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Dimethyl acetylenedicarboxylate → HCID 86609166, 화합물

HRID 1375558
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HRID 1375558 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:15][C@H:14]([O:16][CH3:17])[CH2:13][C@H:12]1[C:18]([NH2:21])=[N:19][OH:20])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:22]([C:28]([O:30][CH3:31])=[O:29])#[C:23][C:24]([O:26][CH3:27])=[O:25]>C(Cl)(Cl)Cl>[CH3:27][O:26][C:24](=[O:25])[C:23]([O:20][N:19]=[C:18]([NH2:21])[C@@H:12]1[CH2:13][C@@H:14]([O:16][CH3:17])[CH2:15][N:11]1[C:9]([O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)=[O:10])=[CH:22][C:28]([O:30][CH3:31])=[O:29]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 12980Dimethyl acetylenedicarboxylateHCID 86609165HCID 86609165, 화합물

생성물 1

HCID 86609166HCID 86609166, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
40 °C

실험 절차

To benzyl-(2S,4R)-2-[amino(hydroxyimino)methyl]-4methoxypyrrolidine-1-carboxylate, dissolved in chloroform, dimethyl acetylendicarboxylate (1.1 eq.) was added. The mixture was refluxed for 1 hour and left stirring at 40° C. overnight. The chloroform was removed in vacuo and the crude product purified by flash chromatography on silica gel (eluent ethyl acetate:petroleum ether=40:60). Two isomers were present in ratio 7:3.

후처리

  1. temperatureThe mixture was refluxed for 1 hour
  2. waitleft
  3. customThe chloroform was removed in vacuo
  4. customthe crude product purified by flash chromatography on silica gel (eluent ethyl acetate:petroleum ether=40:60)

출처 및 근거

ORD 기록
ord-e7e27cb1ac674113ad5412a074ba314f
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07169780B2

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