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

HRID 1895904노트

반응식

HRID 1895904 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-32d0a415837849fa861e8ad8bd22954a
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518934B2

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