Process for the preparation of 3,4,9,10-perylenetetracarboxylic acid diimide
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C07D-221/14
C07D-471/06
출원번호
US-0601862
(1984-04-19)
우선권정보
DE-3314430 (1983-04-21); DE-3345810 (1983-12-17)
발명자
/ 주소
Spietschka Ernst (Idstein/Taunus DEX) Urban Manfred (Wiesbaden DEX)
출원인 / 주소
Hoechst Aktiengesellschaft (DEX 03)
인용정보
피인용 횟수 :
4인용 특허 :
0
초록▼
Preparation of 3,4,9,10-perylenetetracarboxylic acid diimide by fusing naphthalene-1,8-dicarboxylic acid imide with potassium hydroxide and sodium acetate to give the alkali metal salt of the leuko compound of 3,4,9,10-perylenetetracarboxylic acid diimide, diluting the melt with water when the react
Preparation of 3,4,9,10-perylenetetracarboxylic acid diimide by fusing naphthalene-1,8-dicarboxylic acid imide with potassium hydroxide and sodium acetate to give the alkali metal salt of the leuko compound of 3,4,9,10-perylenetetracarboxylic acid diimide, diluting the melt with water when the reaction has ended and oxidizing the leuko form to give the 3,4,9,10-perylenetetracarboxylic acid diimide, by a procedure which comprises (a) applying a vacuum of less than 100 mm Hg before the naphthalene-1,8-dicarboxylic acid imide is introduced into the potassium hydroxide/sodium acetate melt, heating the potassium hydroxide/sodium acetate mixture to 200°-300°C. and dehydrating it such that the melt is still stirrable at 200°-220°C., and then introducing the naphthalene-1,8-dicarboxylic acid imide or its sodium or potassium salt into the melt at 200°-220°C. under normal pressure and heating the mixture at 250°-300°C. in the absence of atmospheric oxygen, or (b) applying a vacuum of less than 100 mm Hg after the naphthalene-1,8-dicarboxylic acid imide or its sodium or potassium salt has been introduced into the potassium hydroxide/sodium acetate melt at 200°-220°C. under normal pressure, heating the mixture to 200°-250°C. and dehydrating it such that the melt is still stirrable at 200°-220°C., and then heating the melt at 250°-300°C. in the absence of atmospheric oxygen, or (c) introducing the sodium or potassium salt of naphthalene-1,8-dicarboxylic acid imide into the potassium hydroxide/sodium acetate melt at 200°-220°C. under normal pressure and heating the melt at 250°-300°C. in the absence of atmospheric oxygen.
대표청구항▼
A process for the preparation of 3,4,9,10-perylenetetracarboxylic acid diimide with a high degree of purity and in a high yield in which yield the amount of 100% 3,4,9,10-perylene-tetracarboxylic acid diimide is comparatively high, by fusing naphthalane-1,8-dicarboxylic acid imide with potassium hyd
A process for the preparation of 3,4,9,10-perylenetetracarboxylic acid diimide with a high degree of purity and in a high yield in which yield the amount of 100% 3,4,9,10-perylene-tetracarboxylic acid diimide is comparatively high, by fusing naphthalane-1,8-dicarboxylic acid imide with potassium hydroxide and sodium acetate to give the alkali metal salt of the leuko compound of 3,4,9,10-perylenetetracarboxylic acid diimide, diluting the melt with water, when the reaction has ended, and oxidizing the leuko form to 3,4,9,10-perylenetetracarboxylic acid diimide, which comprises (a) applying a vacuum of less than 100 mm Hg before the naphthalene-1,8-dicarboxylic acid imide is introduced into the potassium hydroxide/sodium acetate melt, heating the potassium hydroxide/sodium acetate mixture to 250°-300°C., and hereby dehydrating this mixture such that the melt obtained is still stirrable at 200°-220°C. under industrial conditions, subsequently introducing the naphthalene-1,8-dicarboxylic acid imide or its sodium or potassium salt into the above melt at 200°-220°C. under normal pressure and heating this melt, in the absence of atmospheric oxygen, at 250°-300°C. until formation of the alkali metal salt of the leuko compound is complete, or (b) applying a vacuum of less than 100 mm Hg after the naphthalene-1,8-dicarboxylic acid imide or its sodium or potassium salt has been introduced into the potassium hydroxide/sodium acetate melt at 200°-220°C. under normal pressure, heating the mixture to 200°-250°C. and hereby dehydrating it such that the melt obtained is still stirrable at 200°-220°C. under industrial conditions, and subsequently heating the melt, in the absence of atmospheric oxygen, at 250°-300°C. until formation of the alkali metal salt of the leuko compound is complete, or (c) introducing the sodium or potassium salt of the naphthalene-1,8-dicarboxylic acid imide into the potassium hydroxide/sodium acetate melt at 200°-220°C. under normal pressure and heating the melt, in the absence of atomospheric oxygen, at 250°-300°C. until the formation of the alkali metal salt of the leuko compound is complete.
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이 특허를 인용한 특허 (4)
Erk, Peter; Schaefer, Simone; Boehm, Arno; Blaschka, Peter; Arms, Harald; Helfer, Willi, Method for converting perylen-3,4:9,10-tetracarboxylic acid diimides into a form suitable for use as a fluorescent dye.
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