Dimethylcarbamoyl Chloride → Trans-3-(4-chlorophenoxy)-4-hydroxy-N,N-dimethyl-1-pyrrolidinecarboxamide

HRID 1381220노트

반응식

HRID 1381220 반응식
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][CH:7]2[CH2:11][NH:10][CH2:9][CH:8]2[OH:12])=[CH:4][CH:3]=1.[CH3:15][N:16]([CH3:20])[C:17](Cl)=[O:18].C(N(CC)CC)C>C(Cl)Cl>[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][C@H:7]2[C@H:8]([OH:12])[CH2:9][N:10]([C:17]([N:16]([CH3:20])[CH3:15])=[O:18])[CH2:11]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 13320209HCID 13320209, 화합물

생성물 1

HCID 13320214Trans-3-(4-chlorophenoxy)-4-hydroxy-N,N-dimethyl-1-pyrrolidinecarboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 3.5 g. of 4-(4-chlorophenoxy)-3-pyrrolidinol, 1.8 g. of dimethylcarbamyl chloride and 1.7 g. of triethylamine in 300 ml of methylene chloride was stirred for 60 hr. The solvent was removed under vacuum, 300 ml of benezene was added and the mixture was refluxed for 2 hr., then filtered. After solvent evaporation, the residue was dissolved in cyclohexane-benzene and charcoaled. The product was then crystallized, collected by filtration and recrystallized from cyclohexane-benzene; m.p. 137°-142° C.

후처리

  1. customThe solvent was removed under vacuum, 300 ml of benezene
  2. additionwas added
  3. temperaturethe mixture was refluxed for 2 hr
  4. filtration, then filtered
  5. customAfter solvent evaporation
  6. dissolutionthe residue was dissolved in cyclohexane-benzene
  7. customThe product was then crystallized
  8. filtrationcollected by filtration
  9. customrecrystallized from cyclohexane-benzene

출처 및 근거

ORD 기록
ord-a1800dec433e46b2aff70c16bb67f4c6
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04585785

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