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

HRID 129646ノート

反応式

HRID 129646 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-ad5fc0c2af754edcbfdc8a065345f3fb
出典データセット
uspto-grants-1995_11
特許番号
US05468877

反応ノート

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