Hydrazine hydrate (1:1) → O-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-4-yl)hydroxylamine

HRID 1895904ノート

反応式

HRID 1895904 の反応式
O.NN.[F:4][C:5]([F:34])([F:33])[C:6]1[CH:7]=[C:8]([S:12]([N:15]2[CH2:20][CH2:19][CH:18]([O:21][N:22]3C(=O)C4C(=CC=CC=4)C3=O)[CH2:17][CH2:16]2)(=[O:14])=[O:13])[CH:9]=[CH:10][CH:11]=1>C(O)C>[F:34][C:5]([F:4])([F:33])[C:6]1[CH:7]=[C:8]([S:12]([N:15]2[CH2:16][CH2:17][CH:18]([O:21][NH2:22])[CH2:19][CH2:20]2)(=[O:14])=[O:13])[CH:9]=[CH:10][CH:11]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 671183862-(1-(3-(Trifluoromethyl)phenylsulfonyl)piperidin-4-yloxy)isoindoline-1,3-dione

生成物 1

HCID 67118429O-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-4-yl)hydroxylamine収率 99.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Hydrazine monohydrate (250 mg, 4.24 mmol) was added to a solution of 2-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-4-yloxy)isoindoline-1,3-dione (1.02 g, 2.24 mmol) in ethanol (10 ml) and stirred at room temperature for 30 minutes. The resulting solid was filtered off and concentrated in vacuo. The residue was triturated with diethyl ether (30 ml), and the resulting solid was filtered off again and concentrated in vacuo to give O-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-4-yl)hydroxylamine (720 mg, 94%) as a white solid: LCMS: 343 [M+1]+.

後処理

  1. filtrationThe resulting solid was filtered off
  2. concentrationconcentrated in vacuo
  3. customThe residue was triturated with diethyl ether (30 ml)
  4. filtrationthe resulting solid was filtered off again
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-32d0a415837849fa861e8ad8bd22954a
出典データセット
uspto-grants-2013_08
特許番号
US08518934B2

反応ノート

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