Ethyl chloroacetate → (2,2-Dimethyl-pyrrolidin-1-yl)-acetic acid ethyl ester

HRID 644080노트

반응식

HRID 644080 반응식
[CH2:1]([O:3][C:4](=[O:7])[CH2:5]Cl)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH3:14][C:15]1([CH3:20])[CH2:19][CH2:18][CH2:17][NH:16]1>C(O)C.C(OCC)C>[CH2:1]([O:3][C:4](=[O:7])[CH2:5][N:16]1[CH2:17][CH2:18][CH2:19][C:15]1([CH3:20])[CH3:14])[CH3:2]

참가 물질

6

반응물 3

HCID 7751Ethyl chloroacetateHCID 11430Potassium CarbonateHCID 4147732,2-Dimethylpyrrolidine

생성물 1

HCID 63219360(2,2-Dimethyl-pyrrolidin-1-yl)-acetic acid ethyl ester수율 61.5%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

Ethylchloroacetate (0.15 ml, 1.37 mmol), potassium carbonate (416 mg, 1.5 mmol) and 2,2-dimethyl-pyrolidine (0.280 mg, 2.06 mmol) were suspended in ethanol (3 ml) and subjected to microwave irradiation at 120° C. for 45 min. The resultant mixture was suspended in diethyl ether (30 ml), extracted with 2M hydrochloric acid (30 ml) and the organic layer discarded. The aqueous layer was treated with a slight excess of 4N sodium hydroxide solution and extracted with diethyl ether (3×30 ml). The organic layers were combined, dried over sodium sulfate, filtered and solvent removed under reduced pressure to afford (2,2-dimethyl-pyrrolidin-1-yl)-acetic acid ethyl ester (156 mg).

후처리

  1. customirradiation at 120° C. for 45 min
  2. extractionextracted with 2M hydrochloric acid (30 ml)
  3. additionThe aqueous layer was treated with a slight excess of 4N sodium hydroxide solution
  4. extractionextracted with diethyl ether (3×30 ml)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customsolvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-7bfcbf497a894ea8867f2117c7808ace
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700634B2

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