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

HRID 1974760ノート

反応式

HRID 1974760 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bdb257a1e95b4e1b90aaa522f3f6adef
出典データセット
uspto-grants-1994_02
特許番号
US05283361

反応ノート

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