Acetic Anhydride → HCID 20301696, 화합물

HRID 2052443노트

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HRID 2052443 반응식
[OH:1][C:2]1[C:12]2[NH:11][CH:10]([O:13][CH3:14])[CH:9]3[CH2:15][CH2:16][CH2:17][N:8]3[C:7](=[O:18])[C:6]=2[CH:5]=[CH:4][C:3]=1[CH3:19].[C:20](OC(=O)C)(=[O:22])[CH3:21]>C(N(CC)CC)C>[C:20]([O:1][C:2]1[C:12]2[NH:11][CH:10]([O:13][CH3:14])[CH:9]3[CH2:15][CH2:16][CH2:17][N:8]3[C:7](=[O:18])[C:6]=2[CH:5]=[CH:4][C:3]=1[CH3:19])(=[O:22])[CH3:21]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 13567453HCID 13567453, 화합물

생성물 1

HCID 20301696HCID 20301696, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

49.3 mg of 2,3,5,10,11,11a-hexahydro-9-hydroxy-11-methoxy-8-methyl-1H-pyrrolo[2,1-C][1,4]benzodiazepin-5-one was suspended in 0.5 ml of 1:1 mixture of triethylamine and acetic anhydride and stirred at 0° to 5° C. for 15 minutes under a stream of nitrogen gas. Thus, 30 mg of 2,3,5,10,11,11a-hexahydro-9-acetoxy-11-methoxy-8-methyl-1H-pyrrolo[2,1-C][1,4]benzodiazepin-5-one was obtained as a colorless powdery product. Recrystallization of the resulting product from acetone-ligroin gave a colorless needle-like crystal having a melting point of 147° to 149.5° C.

출처 및 근거

ORD 기록
ord-1dfaeb7d274e4b05ac5eb09ac9d78637
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04185016

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