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

HRID 1974762ノート

反応式

HRID 1974762 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][OH:20])=[CH:4][CH:3]=1.C[Si]([N:25]=[C:26]=[O:27])(C)C.Cl>O1CCOCC1>[OH:20][N:19]([CH2:18][CH:17]=[CH:16][C:10]1[C:11]([F:15])=[CH:12][CH:13]=[CH:14][C:9]=1[S:8][C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=1)[C:26]([NH2:25])=[O:27]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 70696Trimethylsilyl isocyanateHCID 53877237N-[3-[2-(4-fluorophenylthio)-6-fluorophenyl]prop-2-enyl]hydroxylamine

生成物 1

HCID 54054261N-hydroxy-N-[3-[2-(4-fluorophenylthio)-6-fluorophenyl]prop-2-enyl]urea

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

N-[3-[2-(4-fluorophenylthio)-6-fluorophenyl]prop-2-enyl]hydroxylamine (0.91 g, 3.1 mmol) is dissolved in 16 ml of dry dioxane. Trimethylsilyl isocyanate (0.36 g, 3.1 mmol) is then added dropwise and the reaction mixture is stirred at room temperature overnight. The reaction mixture is poured into 1N HCl solution and then extracted twice with diethyl ether. The extracts are washed with water and then with brine and dried over K2CO3 to afford the crude product. Recrystallization from ethyl acetate afforded the subtitle compound.

後処理

  1. extractionextracted twice with diethyl ether
  2. washThe extracts are washed with water
  3. dry with materialwith brine and dried over K2CO3
  4. customto afford the crude product
  5. customRecrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-e8a00009d2e14fceb9c1b9cccd241fb8
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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