4-(2-Chloroethyl)benzoic acid → 5,10,11,11a-tetrahydro-9-[2-(4-carboxyphenyl)-ethoxy]-11-methoxy-8-methyl-5-oxo-1H-pyrrolo-[2,1-C][1,4]benzodiazepine-2-acrylamide

HRID 279773노트

반응식

HRID 279773 반응식
[OH:1][C:2]1[C:12]2[NH:11][CH:10]([O:13][CH3:14])[CH:9]3[CH2:15][CH:16]=[CH:17][N:8]3[C:7](=[O:18])[C:6]=2[CH:5]=[CH:4][C:3]=1[CH3:19].[C:20]([C:23]1[CH:28]=[CH:27][C:26]([CH2:29][CH2:30]Cl)=[CH:25][CH:24]=1)([OH:22])=[O:21]>N1C=CC=CC=1>[C:20]([C:23]1[CH:28]=[CH:27][C:26]([CH2:29][CH2:30][O:1][C:2]2[C:12]3[NH:11][CH:10]([O:13][CH3:14])[CH:9]4[CH2:15][C:16]([CH:15]=[CH:9][C:10]([NH2:11])=[O:13])=[CH:17][N:8]4[C:7](=[O:18])[C:6]=3[CH:5]=[CH:4][C:3]=2[CH3:19])=[CH:25][CH:24]=1)([OH:22])=[O:21]

참가 물질

4

반응물 2

HCID 887124-(2-Chloroethyl)benzoic acidHCID 233225535,10,11,11a-tetrahydro-9-hydroxy-11-methoxy-8-methyl-5-oxo-1H-pyrrolo-[2,1-C][1,4]benzodiazepine

생성물 1

HCID 539697195,10,11,11a-tetrahydro-9-[2-(4-carboxyphenyl)-ethoxy]-11-methoxy-8-methyl-5-oxo-1H-pyrrolo-[2,1-C][1,4]benzodiazepine-2-acrylamide

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

In 120 ml of pyridine were reacted 300 mg of 5,10,11,11a-tetrahydro-9-hydroxy-11-methoxy-8-methyl-5-oxo-1H-pyrrolo-[2,1-C][1,4]benzodiazepine and 1 g of 1-(4-carboxyphenyl)-2-chloroethane, for 12 hr at 50° C. After completion of the reaction, purification and recrystallization were conducted in the same manner as in Example 14 to obtain a light yellow crystal of 5,10,11,11a-tetrahydro-9-[2-(4-carboxyphenyl)-ethoxy]-11-methoxy-8-methyl-5-oxo-1H-pyrrolo-[2,1-C][1,4]benzodiazepine-2-acrylamide having a melting point of 193° to 195° C. Further, this product was converted to a corresponding sodium salt in the same manner as in Example 14. The yield of the sodium salt was 350 mg.

후처리

  1. customAfter completion of the reaction, purification and recrystallization

출처 및 근거

ORD 기록
ord-56f08a1ef6fd495c87b48f0cc5f2e6d7
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587052

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