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

HRID 1974762노트

반응식

HRID 1974762 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e8a00009d2e14fceb9c1b9cccd241fb8
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05283361

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