Hydrochloric Acid → N-[3-[2-(4-fluorophenylthio)-6-fluorophenyl]prop-2-enyl]hydroxylamine

HRID 1974761ノート

反応式

HRID 1974761 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[C:10]=2[CH:16]=[CH:17][CH2:18][NH:19][O:20]C2CCCCO2)=[CH:4][CH:3]=1.Cl>CO>[F:1][C:2]1[CH:3]=[CH:4][C:5]([S:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[C:10]=2[CH:16]=[CH:17][CH2:18][NH:19][OH:20])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 54561379N-[3-[2-(4-fluorophenylthio)-6-fluorophenyl]prop-2-enyl]-O-tetrahydropyranyl hydroxylamine

生成物 1

HCID 53877237N-[3-[2-(4-fluorophenylthio)-6-fluorophenyl]prop-2-enyl]hydroxylamine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

N-[3-[2-(4-fluorophenylthio)-6-fluorophenyl]prop-2-enyl]-O-tetrahydropyranyl hydroxylamine (1.26 g, 3.34 mmol) is dissolved in 17 ml of methanol and cooled in an ice bath. Concentrated HCl (1.7 ml) is then added dropwise and the reaction mixture is stirred overnight at room temperature. The reaction mixture is evaporated to dryness and then slurried in saturated NaHCO3 solution and extracted twice with diethyl ether. The extracts are washed with water and then brine and dried over K2CO3 to afford the subtitle compound.

後処理

  1. temperaturecooled in an ice bath
  2. customThe reaction mixture is evaporated to dryness
  3. extractionextracted twice with diethyl ether
  4. washThe extracts are washed with water
  5. dry with materialbrine and dried over K2CO3

出典と根拠

ORDレコード
ord-112f0cc4e1cc4a1c8e8186e9d47957e2
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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