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Dimethylformamide dimethyl acetal → (Z)-tert-butyl 3-((dimethylamino)methylene)-4-oxopyrrolidine-1-carboxylate

HRID 225568
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HRID 225568 반응식
[C:1]([N:8]1[CH2:12][CH2:11][C:10](=[O:13])[CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].CO[CH:16](OC)[N:17]([CH3:19])[CH3:18]>CN(C)C=O>[C:4]([O:3][C:1]([N:8]1[CH2:9][C:10](=[O:13])/[C:11](=[CH:16]\[N:17]([CH3:19])[CH3:18])/[CH2:12]1)=[O:2])([CH3:7])([CH3:6])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 471360Tert-butyl 3-oxopyrrolidine-1-carboxylate

생성물 1

HCID 56971730(Z)-tert-butyl 3-((dimethylamino)methylene)-4-oxopyrrolidine-1-carboxylate수율 90%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 13.5 mmol N-BOC-3-pyrrolidone and 13.5 mmol N,N-dimethylformamide-dimethylacetal in 50 ml N,N-dimethylformamide was hold overnight at 60° C. The reaction mixture was quenched by addition of 50 ml water and extracted 3 times with ethyl acetate. The extract was dried over magnesium sulfate and concentrated to give the crude title compound as a yellowish oil. Yield=90%. MS (m/e): 241.4 ([M+H]+, 100%).

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후처리

  1. customThe reaction mixture was quenched by addition of 50 ml water
  2. extractionextracted 3 times with ethyl acetate
  3. dry with materialThe extract was dried over magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9375a58ecd2242a4a6def5cdde1944ef
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07557114B2

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