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Hydrochloric Acid → ethyl(E)-3-[1-(4-benzyloxybenzyl)-4-phenyl-3-pyrrolyl]propenoate

HRID 350030
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인쇄 미리보기

반응식

HRID 350030 반응식
[H-].[Na+].[CH2:3]([O:10][C:11]1[CH:30]=[CH:29][C:14]([CH2:15][N:16]2[CH:20]=[C:19]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:18]([CH:27]=O)=[CH:17]2)=[CH:13][CH:12]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C(OP([CH2:39][C:40]([O:42][CH2:43][CH3:44])=[O:41])(OCC)=O)C.Cl>CN(C)C=O>[CH2:3]([O:10][C:11]1[CH:30]=[CH:29][C:14]([CH2:15][N:16]2[CH:20]=[C:19]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[C:18](/[CH:27]=[CH:39]/[C:40]([O:42][CH2:43][CH3:44])=[O:41])=[CH:17]2)=[CH:13][CH:12]=1)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 13345Triethyl phosphonoacetateHCID 24758Sodium hydrideHCID 230249941-(4-Benzyloxybenzyl)-4-phenylpyrrole-3-carbaldehyde

생성물 1

HCID 69421069ethyl(E)-3-[1-(4-benzyloxybenzyl)-4-phenyl-3-pyrrolyl]propenoate수율 94.1%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

Sodium hydride (60%, oily, 2.13 g) was added to a mixture of 1-(4-benzyloxybenzyl)-4-phenylpyrrole-3-carbaldehyde (18.00 g), ethyl diethylphosphonoacetate (12.09 g) and N,N-dimethylformamide (150 ml) at 0° C., and the mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into dilute hydrochloric acid, which was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution, dried (MgSO4), and then concentrated. The residue was subjected to silica gel column chromatography, and ethyl(E)-3-[1-(4-benzyloxybenzyl)-4-phenyl-3-pyrrolyl]propenoate (20.16 g, yield: 94%) was obtained as colorless crystals from the fraction eluted with ethyl acetate-hexane (1:4, volume ratio). This was recrystallized from ethyl acetate-hexane. Melting point: 111–112° C.

후처리

  1. extractionwas extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated aqueous sodium chloride solution
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e921731164064093bfffcbe542b428f8
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07179823B1

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