Acetic Anhydride → Acetamide, N-(4-(7-acetyl-8,9-dihydro-8-methyl-7H-1,3-dioxolo(4,5-h)(2,3)benzodiazepin-5-yl)phenyl)-

HRID 2210507

반응식

HRID 2210507 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:14]3[CH:15]=[C:16]4[O:21][CH2:20][O:19][C:17]4=[CH:18][C:13]=3[CH2:12][CH:11]([CH3:22])[N:10]([C:23](=[O:25])[CH3:24])[N:9]=2)=[CH:4][CH:3]=1.[C:26](OC(=O)C)(=[O:28])[CH3:27]>>[C:26]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:14]3[CH:15]=[C:16]4[O:21][CH2:20][O:19][C:17]4=[CH:18][C:13]=3[CH2:12][CH:11]([CH3:22])[N:10]([C:23](=[O:25])[CH3:24])[N:9]=2)=[CH:4][CH:3]=1)(=[O:28])[CH3:27]

참가 물질

3

반응물 2

HCID 7918Acetic AnhydrideHCID 126756Gyki-53405

생성물 1

HCID 3072691Acetamide, N-(4-(7-acetyl-8,9-dihydro-8-methyl-7H-1,3-dioxolo(4,5-h)(2,3)benzodiazepin-5-yl)phenyl)-

실험 절차

1.3 g (4.4 mmol) of 1-(4-aminophenyl)-3-acetyl-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine were stirred at 20°-25° C. with 5 ml of acetic anhydride for one hour, then the yellow solution was poured into 100 g of ice-water and stirred until the decomposition of the excess anhydride became complete. The precipitate formed was filtered, washed with 3×10 ml of distilled water and dried to give 1.6 g of raw product. After recrystallization from 20 ml of benzene 1.50 g (89.85%) of the aimed product were obtained, m.p.: 158°-160° C. (decomp.).

후처리

  1. customThe precipitate formed
  2. filtrationwas filtered
  3. washwashed with 3×10 ml of distilled water
  4. customdried

출처 및 근거

ORD 기록
ord-b8aaddea27be494cb4ac9a4254081a4a
출처 데이터셋
uspto-grants-1995_10
특허 번호
US05459137

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