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

HRID 1447956

反応式

HRID 1447956 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8058Hexane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5672a21d33ce40b3b7154d76b3ba6695
出典データセット
uspto-grants-1979_12
特許番号
US04179276

関連ノート

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