Dichloromethane → Trifluoromethyl 1-chloro-N-(p-chlorobenzyl)thioformimidate

HRID 129646

반응식

HRID 129646 반응식
[F:1][C:2]([F:6])([F:5])[S:3]Cl.[Cl:7][C:8]1[CH:16]=[CH:15][C:11]([CH2:12][N+:13]#[C-:14])=[CH:10][CH:9]=1.C(Cl)[Cl:18]>>[Cl:18][C:14](=[N:13][CH2:12][C:11]1[CH:15]=[CH:16][C:8]([Cl:7])=[CH:9][CH:10]=1)[S:3][C:2]([F:6])([F:5])[F:1]

참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 67900Methanesulfenyl chloride, trifluoro-HCID 27574091-Chloro-4-(isocyanomethyl)benzene

생성물 1

HCID 18930385Trifluoromethyl 1-chloro-N-(p-chlorobenzyl)thioformimidate수율 68%

실험 절차

Trifluoromethylsulfenyl chloride (4.0 g, 0.03 mol) is bubbled over 30 minutes into a solution of 4-chlorobenzylisonitrile (3.0 g, 0.02 mol) in methylene chloride, causing the formation of a white precipitate. The suspension is stirred for 16 hours at room temperature and filtered to remove solids. The white filter cake is washed with methylene chloride and solvent is removed under reduced pressure to obtain an amber oil. Bulb-to-bulb distillation of the oil (90°-100° C., 0.05 mmHg) gives the title product as a colorless oil (3.9 g, 68%).

후처리

  1. filtrationfiltered
  2. customto remove solids
  3. washThe white filter cake is washed with methylene chloride and solvent
  4. customis removed under reduced pressure
  5. customto obtain an amber oil
  6. distillationBulb-to-bulb distillation of the oil (90°-100° C., 0.05 mmHg)

출처 및 근거

ORD 기록
ord-ad5fc0c2af754edcbfdc8a065345f3fb
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05468877

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