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 279773ノート

反応式

HRID 279773 の反応式
[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]

参加物

4

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  1. customAfter completion of the reaction, purification and recrystallization

出典と根拠

ORDレコード
ord-56f08a1ef6fd495c87b48f0cc5f2e6d7
出典データセット
uspto-grants-1986_05
特許番号
US04587052

反応ノート

読み込み中…