Hydrochloric Acid → Methyl 2-(1-(3,4-dichlorophenylsulfonyl)pyrrolidin-2-yl)acetate

HRID 1642143노트

반응식

HRID 1642143 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([S:9](Cl)(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].[CH3:13][O:14][C:15](=[O:22])[CH2:16][CH:17]1[CH2:21][CH2:20][CH2:19][NH:18]1.Cl>C(Cl)Cl.C(N(CC)CC)C>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([N:18]2[CH2:19][CH2:20][CH2:21][CH:17]2[CH2:16][C:15]([O:14][CH3:13])=[O:22])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 7383Benzenesulfonyl chloride, 3,4-dichloro-HCID 5323862Methyl 2-(pyrrolidin-2-yl)acetate

생성물 1

HCID 66756029Methyl 2-(1-(3,4-dichlorophenylsulfonyl)pyrrolidin-2-yl)acetate

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 8471Triethylamine용매

실험 절차

A solution of 3,4-dichlorobenzenesulfonyl chloride (1.88 g, 7.65 mmol) in DCM (15 ml) was added dropwise at 0° C. to a solution, cooled to 0° C., of pyrrolidin-2-ylacetic acid methyl ester (1.5 g, 8.4 mmol) in DCM (33 ml) and triethylamine was (2.66 ml, 21 mmol), and stirring was then carried out for 90 minutes at room temperature. 0.5 M HCl (20 ml) was then added, and stirring was carried out for a further 15 minutes. The organic phase was separated, washed with water and dried over sodium sulfate. The solvent was removed using a rotary evaporator and the product was used in the next stage without being purified further. Yield: 2.1 g (77%)

후처리

  1. stirringstirring
  2. waitwas carried out for a further 15 minutes
  3. customThe organic phase was separated
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. customThe solvent was removed
  7. customa rotary evaporator
  8. customwithout being purified further

출처 및 근거

ORD 기록
ord-afc8ef7011c644f5a030ab3b2fe811ff
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119633B2

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