4-Nitrobenzaldehyde → HCID 3565458, 화합물

HRID 2350836노트

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HRID 2350836 반응식
CC1C=CC=C(C)N=1.[N+](C1C=CC(C=O)=CC=1)([O-])=[O:10].[N+:20]([C:23]1[CH:47]=[CH:46][C:26]([CH:27]=[CH:28][C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([CH:35]=[CH:36][C:37]3[CH:42]=[CH:41][C:40]([N+:43]([O-:45])=[O:44])=[CH:39][CH:38]=3)[N:30]=2)=[CH:25][CH:24]=1)([O-:22])=[O:21].ClC1C=CC=C(C(OO)=O)C=1>ClCCl>[N+:20]([C:23]1[CH:47]=[CH:46][C:26]([CH:27]=[CH:28][C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([CH:35]=[CH:36][C:37]3[CH:42]=[CH:41][C:40]([N+:43]([O-:45])=[O:44])=[CH:39][CH:38]=3)[N+:30]=2[O-:10])=[CH:25][CH:24]=1)([O-:22])=[O:21]

참가 물질

6

반응물 4

HCID 5414-NitrobenzaldehydeHCID 79372,6-LutidineHCID 70297m-Chloroperbenzoic acidHCID 5143617Pyridine, 2,6-bis[2-(4-nitrophenyl)ethenyl]-

생성물 1

HCID 3565458HCID 3565458, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

More specifically, the synthesizing procedure is as follows. 2,6-dimethylpyridine or a substituted product thereof, is reacted with p-nitrobenzenealdehyde or a substituted product according to a method described, for example, in Journal of Organic Chemistry, vol. 15, P. 1184 (1950) to synthesize 2,6-di(p-nitrostyryl)pyridine (K). 30 g of this nitro compound is reacted wtih 27 g of m-chloroperbenzoic acid in three liter of dichloromethane to obtain 24 g of 2,6-di(p-nitrostyryl)pyridine-N-oxide. 24 g of this pyridine-N-oxide is reacted with 90 g of sodium sulfide in a solution mixed four liter of water with four liter of ethanol to reduce nitro group selectively and form 18 g of 2,6-di(p-aminostyryl)pyridine-N-oxide (M). The N-oxide amino compound is converted into a diazo compound according to a conventional method, and thereby tetrazonium salt is isolated as 15 g of hydroborofluoric salt (N). 5.0 g of the tetrazonium salt (N) and 5.0 g of 2-hydroxy-3-phenylcarbamoylnaphthalene (O) were dissolved in one liter of DMF, to which aqueous sodium acetate solution (7 g/100 ml) was added to perform coupling reaction. After two hours of stirring, the resultant crystals were separated by filtration, and the crystals were rinsed three times respectively with five liter water, three times respectively with five liter THF, then dried, to obtain 4.0 g of the final product, azo compound (P - 1).

후처리

  1. customMore specifically, the synthesizing procedure

출처 및 근거

ORD 기록
ord-c5b8b680dc3e4b3b953b39341ab9de81
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04871633

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