Acetic Anhydride → HCID 86758535, 화합물

HRID 989638노트

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HRID 989638 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[NH:13][CH:12]([CH2:14][C:15]([O:17][CH3:18])=[O:16])[C:11](=[O:19])[N:10]([CH3:20])[CH2:9][C:8]=2[CH:21]=1)([OH:3])=[O:2].[C:22](OC(=O)C)(=[O:24])[CH3:23]>C(O)(=O)C>[C:22]([N:13]1[C:7]2[CH:6]=[CH:5][C:4]([C:1]([OH:3])=[O:2])=[CH:21][C:8]=2[CH2:9][N:10]([CH3:20])[C:11](=[O:19])[CH:12]1[CH2:14][C:15]([O:17][CH3:18])=[O:16])(=[O:24])[CH3:23]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 23505570Methyl 7-carboxy-2,3,4,5-tetrahydro-4-methyl-3-oxo-1h-1,4-benzodiazepine-2-acetate

생성물 1

HCID 86758535HCID 86758535, 화합물수율 78%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Methyl (±)-7-carboxy-4-methyl-3-oxo-2,3,4,5-tetrahydro-1H-1,4-benzodiazepine-2-acetate (2.0 g, 8.6 mmol), acetic anhydride (25 mL) and acetic acid (1 mL) were heated to reflux. After 48 h, the reaction was concentrated, and the residue was diluted with H2O (20 mL) and MeOH (15 mL). The resulting solution was concentrated to give the tide compound (1.8 g, 78%): 1H NMR (400 MHz, DMSO-d6) δ1.7-1.8 (s, 3H), 2.2-2.6 (m, 2H), 2.9-3.0 (s, 3H), 3.5-3.6 (s, 3H), 4.2-4.3 (d, 1H), 4.7-4.8 (d, 1H), 5.8-5.9 (t, 1H), 7.5-7.6 (d, 1H), 7.9-8.0 (dd, 1H), 8.1-8.2 (d, 1H); MS (ES) m/e 335.0 (M+H)+.

후처리

  1. concentrationthe reaction was concentrated
  2. additionthe residue was diluted with H2O (20 mL) and MeOH (15 mL)
  3. concentrationThe resulting solution was concentrated

출처 및 근거

ORD 기록
ord-421df1a9e3df4e5f86ec15020b8a258b
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06458784B1

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