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Dimethylformamide dimethyl acetal → HCID 67065831, 화합물

HRID 241551
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인쇄 미리보기

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HRID 241551 반응식
[C:1]([N:20]1[CH2:24][CH2:23][C:22](=[O:25])[CH2:21]1)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CO[CH:28](OC)[N:29]([CH3:31])[CH3:30]>CN(C=O)C>[CH3:28][N:29]([CH:31]=[C:23]1[CH2:24][N:20]([C:1]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:21][C:22]1=[O:25])[CH3:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 67065856HCID 67065856, 화합물

생성물 1

HCID 67065831HCID 67065831, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A suspension of 1-tritylpyrrolidin-3-one (4.9 g) from Step A in anhydrous DMF (36.0 mL) was dissolved by heating at 80° C. under nitrogen for 10 min. The clear solution was treated with N,N-dimethylformamide dimethyl acetal (18.0 mL) and heated at 80° C. for 12 h. The resulting dark brown solution was evaporated under reduced pressure. The residue was chromatographed on a Biotage® system (silica gel, gradient from 50% to 100% ethyl acetate in hexanes) to yield the title compound. LC-MS=243.1 (M+1).

후처리

  1. dissolutionwas dissolved
  2. temperatureheated at 80° C. for 12 h
  3. customThe resulting dark brown solution was evaporated under reduced pressure
  4. customThe residue was chromatographed on a Biotage® system (silica gel, gradient from 50% to 100% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-ffdb3cd4966d46e7a54066ec3bde00b4
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08653059B2

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