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Nitromethane → HCID 22236902, 화합물

HRID 1743977
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HRID 1743977 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]([CH3:14])=[CH:8][C:9]([O:11][CH2:12][CH3:13])=[O:10].[N+:15]([CH3:18])([O-:17])=[O:16].C1CCN2C(=NCCC2)CC1>C(#N)C>[CH3:14][C:7]([C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=1)([CH2:18][N+:15]([O-:17])=[O:16])[CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6375NitromethaneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 69594025Ethyl 3-(pyridin-2-yl)but-2-enoate

생성물 1

HCID 22236902HCID 22236902, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 6 g of the compound obtained in Step 1, 3.36 ml of nitromethane and 4.26 ml of DBU dissolved in 120 ml of acetonitrile was heated to reflux for 36 hours. After the reaction was completed, the reaction solution was distilled under reduced pressure. The residue thus obtained was purified by a silica gel column chromatography using a mixture of ethyl acetate and n-hexane of 1:9 to obtain 1.8 g of the title compound as a syrup.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 36 hours
  3. distillationthe reaction solution was distilled under reduced pressure
  4. customThe residue thus obtained
  5. customwas purified by a silica gel column chromatography
  6. additiona mixture of ethyl acetate and n-hexane of 1:9

출처 및 근거

ORD 기록
ord-995470827d67461cbbf0be5af4c91273
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07012144B2

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