Water → N-[3-[2-(4-fluorophenylthio)-6-fluorophenyl]prop-2-enyl]-O-tetrahydropyranyl hydroxylamine

HRID 1974760노트

반응식

HRID 1974760 반응식
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][NH2:8].[F:9][C:10]1[CH:15]=[CH:14][C:13]([S:16][C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([F:23])[C:18]=2[CH:24]=[CH:25][CH2:26]Br)=[CH:12][CH:11]=1.O.CCCCCC.C(OCC)(=O)C>CN(C=O)C>[F:9][C:10]1[CH:15]=[CH:14][C:13]([S:16][C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([F:23])[C:18]=2[CH:24]=[CH:25][CH2:26][NH:8][O:7][CH:2]2[CH2:3][CH2:4][CH2:5][CH2:6][O:1]2)=[CH:12][CH:11]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 5142091O-(Tetrahydropyran-2-yl)hydroxylamineHCID 21226206Ethyl acetate hexaneHCID 540068731-[2-(4-Fluorophenylthio)-6-fluorophenyl]3-bromoprop-1-ene

생성물 1

HCID 54561379N-[3-[2-(4-fluorophenylthio)-6-fluorophenyl]prop-2-enyl]-O-tetrahydropyranyl hydroxylamine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

O-tetrahydropyranylhydroxylamine (2.88 g, 24.6 mmol) is dissolved in 15 ml of dry DMF. A solution of 1-[2-(4-fluorophenylthio)-6-fluorophenyl]3-bromoprop-1-ene (2.80 g, 8.2 mmol) in 6 ml of DMF is added and the reaction is stirred for 4 hours at room temperature. The reaction mixture is poured into 200 ml of water and then extracted twice with diethyl ether. The extracts are washed three times with water and then with brine and dried over MgSO4 to afford the crude product. Chromatography on silica gel eluting with 5:1 hexane/ethyl acetate afforded the subtitle compound.

후처리

  1. extractionextracted twice with diethyl ether
  2. washThe extracts are washed three times with water
  3. dry with materialwith brine and dried over MgSO4
  4. customto afford the crude product

출처 및 근거

ORD 기록
ord-bdb257a1e95b4e1b90aaa522f3f6adef
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05283361

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