Methyl Isocyanate → Trans-3-{[(methylamino)carbonyl]oxy}-4-(4-chlorophenoxy)-N,N-dimethyl-1-pyrrolidinecarboxamide

HRID 1262598노트

반응식

HRID 1262598 반응식
[Cl:1][C:2]1[CH:19]=[CH:18][C:5]([O:6][C@H:7]2[C@H:11]([OH:12])[CH2:10][N:9]([C:13]([N:15]([CH3:17])[CH3:16])=[O:14])[CH2:8]2)=[CH:4][CH:3]=1.[CH3:20][N:21]=[C:22]=[O:23]>C(Cl)Cl>[CH3:20][NH:21][C:22]([O:12][C@H:11]1[C@H:7]([O:6][C:5]2[CH:18]=[CH:19][C:2]([Cl:1])=[CH:3][CH:4]=2)[CH2:8][N:9]([C:13]([N:15]([CH3:17])[CH3:16])=[O:14])[CH2:10]1)=[O:23]

참가 물질

4

반응물 2

HCID 12228Methyl IsocyanateHCID 13320214Trans-3-(4-chlorophenoxy)-4-hydroxy-N,N-dimethyl-1-pyrrolidinecarboxamide

생성물 1

HCID 13320218Trans-3-{[(methylamino)carbonyl]oxy}-4-(4-chlorophenoxy)-N,N-dimethyl-1-pyrrolidinecarboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 1.0 g. (0.003 mole) of trans-3-(4-chlorophenoxy)-4-hydroxy-N,N-dimethyl-1-pyrrolidinecarboxamide and 1.0 g. (0.02 mole) of methylisocyanate in 20 ml. of methylene chloride was let stand at ambient temperature for 48 hr. The solution was concentrated to give an oil which crystallized upon standing. The solid was recrystallized from benzene-cyclohexane to yield 0.6 g. (50%) of white solid, m.p. 132°-134° C.

후처리

  1. concentrationThe solution was concentrated
  2. customto give an oil which
  3. customcrystallized
  4. customThe solid was recrystallized from benzene-cyclohexane
  5. customto yield 0.6 g

출처 및 근거

ORD 기록
ord-87023a7aba704f5f9665856df15adfa6
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04452809

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