Hydrazine hydrate (1:1) → HCID 178453872、化合物

HRID 133134

反応式

HRID 133134 の反応式
O.[NH2:2][NH2:3].[F:4][C:5]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:6]=1[C@H:12]1[CH2:18][NH:17][C:16](=S)[C@H:15]([NH:20][C:21](=[O:27])[O:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:14][CH2:13]1>CO>[F:4][C:5]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:6]=1[C@H:12]1[CH2:18][NH:17][C:16](=[N:2][NH2:3])[C@H:15]([NH:20][C:21](=[O:27])[O:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:14][CH2:13]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 59734935tert-Butyl (3R,6S)-6-(2,3-difluorophenyl)-2-thioxoazepan-3-ylcarbamate

生成物 1

HCID 178453872HCID 178453872、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Hydrazine monohydrate (2.23 mL, 46.0 mmol) was added to a solution of tert-butyl (3R,6S)-6-(2,3-difluorophenyl)-2-thioxoazepan-3-ylcarbamate (546 mg, 1.53 mmol) in methanol (25 mL). After 30 min, the mixture was concentrated under reduced pressure. Saturated aqueous NaHCO3 was added and the mixture was extracted with CH2Cl2 (3×). The combined organic extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure to give the title compound. MS: m/z=355 (M+1).

後処理

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionSaturated aqueous NaHCO3 was added
  3. extractionthe mixture was extracted with CH2Cl2 (3×)
  4. dry with materialThe combined organic extracts were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-613e104c280649e1957dea697c6cc6a3
出典データセット
uspto-grants-2008_06
特許番号
US07390798B2

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