HCID 57612764, 화합물 → HCID 57612839, 화합물

HRID 1668417노트

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HRID 1668417 반응식
[CH2:1]([NH:9][C:10]([C@H:12]1[N:17]2[C:18](=[O:35])[C@@H:19]([N:24]3C(=O)C4C(=CC=CC=4)C3=O)[CH2:20][CH2:21][C:22](=[O:23])[N:16]2[CH2:15][CH2:14][CH2:13]1)=[O:11])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>C(O)C>[CH2:1]([NH:9][C:10]([C@H:12]1[N:17]2[C:18](=[O:35])[C@@H:19]([NH2:24])[CH2:20][CH2:21][C:22](=[O:23])[N:16]2[CH2:15][CH2:14][CH2:13]1)=[O:11])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

3

반응물 1

HCID 57612764HCID 57612764, 화합물

생성물 1

HCID 57612839HCID 57612839, 화합물수율 99.5%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

To a mixture/suspension of (1S,9S)-9-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-6,10-dioxo-octahydro-pyridazino[1,2-a][1,2]diazepine-1-carboxylic acid phenethyl-amide (310 mg, 0.70 mmol) and hydrozinehydrate (70 mg, 1.40 mmol) in ethanol (10 mL) is stirred at 60° C. for 2 hours. After cooled to room temperature and concentrated, the reaction mixture is purified by chromatography (CH2Cl2/MeOH:97/3) to give (1S,9S)-9-amino-6,10-dioxo-octahydro-pyridazino[1,2-a][1,2]diazepine-1-carboxylic acid phenethyl-amide (240 mg, 99%) as white solid. (NMR and MS data confirmed, U-3133-67).

후처리

  1. temperatureAfter cooled to room temperature
  2. concentrationconcentrated
  3. customthe reaction mixture is purified by chromatography (CH2Cl2/MeOH:97/3)

출처 및 근거

ORD 기록
ord-28c15c375d0a459f846b776fa2812bd2
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989441B2

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