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Triethylamine → HCID 22922595, 화합물

HRID 2258547
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HRID 2258547 반응식
[NH2:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][N:7]2[C:11]3[CH:12]=[CH:13][C:14]([O:16][CH2:17][CH3:18])=[CH:15][C:10]=3[N:9]([CH:19]3[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)[C:8]2=[O:25])=[C:4]([O:28][CH3:29])[CH:3]=1.Cl[CH2:31]/[CH:32]=[CH:33]\[CH2:34]Cl.C(N(CC)CC)C>CN(C=O)C>[CH:19]1([N:9]2[C:10]3[CH:15]=[C:14]([O:16][CH2:17][CH3:18])[CH:13]=[CH:12][C:11]=3[N:7]([CH2:6][C:5]3[CH:26]=[CH:27][C:2]([N:1]4[CH:34]=[CH:33][CH:32]=[CH:31]4)=[CH:3][C:4]=3[O:28][CH3:29])[C:8]2=[O:25])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 64321151,4-Dichloro-cis-2-buteneHCID 22922550HCID 22922550, 화합물

생성물 1

HCID 22922595HCID 22922595, 화합물수율 44.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1 g of the compound obtained in Example 6, 1 g of cis-1,4-dichloro-2-butene and 1 ml of triethylamine in 20 ml of DMF is heated at reflux for 1 hour 30 minutes under nitrogen atmosphere. After cooling, the reaction mixture is poured into a water/ice mixture, extracted with EtOAc, the organic phase is washed with water and dried over Na2SO4, and the solvent is evaporated off under vacuum. The residue is chromatographed on silica, eluting with DCM. 0.5 g of the expected product is obtained.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 1 hour 30 minutes under nitrogen atmosphere
  3. temperatureAfter cooling
  4. extractionextracted with EtOAc
  5. washthe organic phase is washed with water
  6. dry with materialdried over Na2SO4
  7. customthe solvent is evaporated off under vacuum
  8. customThe residue is chromatographed on silica
  9. washeluting with DCM

출처 및 근거

ORD 기록
ord-dba2a0c685544285b56b1950320891f2
출처 데이터셋
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05661169

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