Triethylamine → 1-Benzyl 3-methyl azetidine-1,3-dicarboxylate

HRID 1958676노트

반응식

HRID 1958676 반응식
Cl.[CH3:2][O:3][C:4]([CH:6]1[CH2:9][NH:8][CH2:7]1)=[O:5].C(N(CC)CC)C.Cl[C:18]([O:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:19]>C(Cl)Cl>[N:8]1([C:18]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:19])[CH2:9][CH:6]([C:4]([O:3][CH3:2])=[O:5])[CH2:7]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 21100040Methyl azetidine-3-carboxylate hydrochloride

생성물 1

HCID 450725021-Benzyl 3-methyl azetidine-1,3-dicarboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

10 g of azetidine-3-carboxylic methyl ester hydrochloride and then 23 ml of triethylamine are added to 150 ml of CH2Cl2. The mixture is cooled and 13.5 g of benzyl chloroformate are added. After leaving overnight at AT, washing is carried out with water and then with HCl (N). After drying, concentrating to dryness and purifying by chromatography on silica (eluent: heptane-AcOEt (gradient from 0% to 50%)), 13.1 g of the expected compound are obtained.

후처리

  1. temperatureThe mixture is cooled
  2. customAfter leaving overnight at AT
  3. washwashing
  4. customAfter drying
  5. concentrationconcentrating to dryness
  6. custompurifying by chromatography on silica (eluent: heptane-AcOEt (gradient from 0% to 50%)), 13.1 g of the expected compound
  7. customare obtained

출처 및 근거

ORD 기록
ord-5fd37fb0346845d19ef9c506ffa14fb7
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410137B2

반응 노트

불러오는 중…