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

HRID 1895900ノート

反応式

HRID 1895900 の反応式
[F:1][C:2]([F:31])([F:30])[C:3]1[CH:4]=[C:5]([S:9]([N:12]2[CH2:17][CH2:16][CH:15]([O:18][N:19]3C(=O)C4C(=CC=CC=4)C3=O)[CH2:14][CH2:13]2)(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1.O.NN>C(O)C>[F:31][C:2]([F:1])([F:30])[C:3]1[CH:4]=[C:5]([S:9]([N:12]2[CH2:13][CH2:14][CH:15]([O:18][NH2:19])[CH2:16][CH2:17]2)(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=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 93%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-4-yloxy)isoindoline-1,3-dione (4.85 g, 10.0 mmol) and hydrazine monohydrate (550 mg, 11.0 mmol) in ethanol (30 ml) was stirred at room temperature for 30 minutes. The resulting solid was filtered off and concentrated in vacuo. The residue was triturated with diethyl ether (80 ml), and the resulting solid was filtered off again and concentrated in vacuo to give O-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-4-yl)hydroxylamine (3.00 g, 93%) as a white solid: LCMS: 325 [M+1]+.

後処理

  1. filtrationThe resulting solid was filtered off
  2. concentrationconcentrated in vacuo
  3. customThe residue was triturated with diethyl ether (80 ml)
  4. filtrationthe resulting solid was filtered off again
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-45e1dd13ad254db988078eb49b10f0a0
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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