Hydrazine → HCID 58550577、化合物

HRID 388859ノート

反応式

HRID 388859 の反応式
[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

参加物

4

反応物 2

HCID 9321HydrazineHCID 58550631HCID 58550631、化合物

生成物 1

HCID 58550577HCID 58550577、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e74dd9bb188e426bb31d49141d084c9f
出典データセット
uspto-grants-2013_02
特許番号
US08377955B2

反応ノート

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