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

HRID 63836노트

반응식

HRID 63836 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d88794e752b94b8592b3cde2735736e0
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447084B2

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