4-Chloro-2-fluorophenyl isocyanate → 3-Carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine

HRID 1447956

반응식

HRID 1447956 반응식
[C:1]([CH:6]1[CH2:11][S:10][CH2:9][CH2:8][NH:7]1)([O:3][CH2:4][CH3:5])=[O:2].[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([N:19]=[C:20]=[O:21])=[C:15]([F:22])[CH:14]=1>CCCCCC.CCOCC>[C:1]([CH:6]1[CH2:11][S:10][CH2:9][CH2:8][N:7]1[C:20]([NH:19][C:16]1[CH:17]=[CH:18][C:13]([Cl:12])=[CH:14][C:15]=1[F:22])=[O:21])([O:3][CH2:4][CH3:5])=[O:2]

참가 물질

5

반응물 2

HCID 45582034-Chloro-2-fluorophenyl isocyanateHCID 13604869Ethyl thiomorpholine-3-carboxylate

생성물 1

HCID 233433973-Carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine수율 87.7%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8058Hexane용매

실험 절차

An emulsion of 14 g of 3-carbethoxythiomorpholine in 50 ml of n-hexane was added dropwise to a solution of 14 g of 4-chloro-2-fluorophenylisocyanate in 60 ml of anhydrous ether at 15° to 28° C. with stirring. A heavy oil formed after the addition. The oil crystallized after stirring at room temperature for 15 min. The precipitate was collected by filtration to give 24.3 g of 3-carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine, m.p. 111.5°-112.5° C.

후처리

  1. customA heavy oil formed
  2. additionafter the addition
  3. customThe oil crystallized
  4. stirringafter stirring at room temperature for 15 min
  5. filtrationThe precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-5672a21d33ce40b3b7154d76b3ba6695
출처 데이터셋
uspto-grants-1979_12
특허 번호
US04179276

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