Hydrazine → HCID 58550577, 화합물

HRID 1890709노트

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HRID 1890709 반응식
[O:1]=[C:2]1[N:10]([CH2:11][O:12][CH2:13][CH2:14][Si:15]([CH3:18])([CH3:17])[CH3:16])[C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:4]2[C@@:3]21[CH2:34][C:21]1=[N:22][C:23]3[CH:24]=[CH:25][C:26]([C:30](OC)=[O:31])=[CH:27][C:28]=3[CH:29]=[C:20]1[CH2:19]2.[NH2:35][NH2:36]>CO>[O:1]=[C:2]1[N:10]([CH2:11][O:12][CH2:13][CH2:14][Si:15]([CH3:17])([CH3:16])[CH3:18])[C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:4]2[C@@:3]21[CH2:34][C:21]1=[N:22][C:23]3[CH:24]=[CH:25][C:26]([C:30]([NH:35][NH2:36])=[O:31])=[CH:27][C:28]=3[CH:29]=[C:20]1[CH2:19]2

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 58550631HCID 58550631, 화합물

생성물 1

HCID 58550577HCID 58550577, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
70 °C

실험 절차

To a solution of methyl (2S)-2′-oxo-1′-{[2-(trimethylsilyl)ethoxy]methyl}-1,1′,2′, 3-tetrahydrospiro[cyclopenta[b]quinoline-2,3′-pyrrolo[2,3-b]pyridine]-7-carboxylate from Step G (317 mg, 0.667 mmol) in MeOH (1 mL) was added hydrazine (1.0 mL, 32 mmol). The reaction was sealed and then heated to 70° C. for 18 hours. After cooling to ambient temperature, the bulk of the solvent was removed in vacuo. The residue was diluted with DCM (50 mL) and water (20 mL). The organics were then successively washed with water, half-saturated brine and brine before being dried over sodium sulfate. The organics were then filtered, concentrated in vacuo to give the title compound. MS: m/z=476 (M+1).

후처리

  1. customThe reaction was sealed
  2. temperatureAfter cooling to ambient temperature
  3. customthe bulk of the solvent was removed in vacuo
  4. additionThe residue was diluted with DCM (50 mL) and water (20 mL)
  5. washThe organics were then successively washed with water, half-saturated brine and brine
  6. dry with materialbefore being dried over sodium sulfate
  7. filtrationThe organics were then filtered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-77543c4397c54d54b5e8af741586555e
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507477B2

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