Dichloromethane → Phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate

HRID 63836ノート

反応式

HRID 63836 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][NH:5][CH2:6][C:7]([F:10])([F:9])[F:8].ClCCl.Cl[C:15]([O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:16]>N1C=CC=CC=1>[Cl:1][CH2:2][CH2:3][CH2:4][N:5]([CH2:6][C:7]([F:10])([F:9])[F:8])[C:15](=[O:16])[O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 15891Phenyl chloroformateHCID 65027041(3-Chloropropyl)(2,2,2-trifluoroethyl)amine

生成物 1

HCID 118046857Phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Into a 500-mL round-bottom flask, was placed (3-chloropropyl)(2,2,2-trifluoroethyl)amine (5 g, 28.48 mmol, 1.00 equiv), dichloromethane (300 mL), TEA (5.8 g, 57.32 mmol, 2.00 equiv), pyridine (0.5 mL). To this was added dropwise phenyl chloroformate (4.4 g, 28.10 mmol, 1.00 equiv) at 0° C. The resulting solution was stirred for 3 h at room temperature. The resulting mixture was washed with 2×100 mL of H2O. The resulting mixture was washed with 2×100 mL of brine. The mixture was dried over sodium sulfate. The resulting mixture was concentrated under vacuum. This resulted in 1.4 g (crude) of phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate as a colorless liquide.

後処理

  1. customInto a 500-mL round-bottom flask, was placed
  2. washThe resulting mixture was washed with 2×100 mL of H2O
  3. washThe resulting mixture was washed with 2×100 mL of brine
  4. dry with materialThe mixture was dried over sodium sulfate
  5. concentrationThe resulting mixture was concentrated under vacuum
  6. customThis resulted in 1.4 g (crude) of phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate as a colorless liquide

出典と根拠

ORDレコード
ord-d88794e752b94b8592b3cde2735736e0
出典データセット
uspto-grants-2016_09
特許番号
US09447084B2

反応ノート

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