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Potassium Carbonate → HCID 67604482, 화합물

HRID 1810
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HRID 1810 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]([CH2:18][C:19]([CH3:22])([CH3:21])[CH3:20])[C:9]([CH:11]=[CH:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:10])=[C:4]([CH:23]([OH:40])[C:24]2[CH:29]=[CH:28][C:27]([O:30][CH2:31][C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)=[CH:26][C:25]=2[O:38][CH3:39])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH2:31]([O:30][C:27]1[CH:28]=[CH:29][C:24]([C@@H:23]2[C:4]3[CH:3]=[C:2]([Cl:1])[CH:7]=[CH:6][C:5]=3[N:8]([CH2:18][C:19]([CH3:21])([CH3:22])[CH3:20])[C:9](=[O:10])[C@@H:11]([CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[O:40]2)=[C:25]([O:38][CH3:39])[CH:26]=1)[C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 67604576ethyl 3-[N-[4-chloro-2-(4-benzyloxy-alpha-hydroxy-2-methoxybenzyl)-phenyl]-N-neopentylcarbamoyl]acrylate

생성물 1

HCID 67604482HCID 67604482, 화합물수율 81.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a mixture of ethyl 3-[N-[4-chloro-2-(4-benzyloxy-α-hydroxy-2-methoxybenzyl)-phenyl]-N-neopentylcarbamoyl]acrylate (12 g), potassium carbonate (5.9 g) and ethanol (150 ml) was stirred for 24 h. After the mixture was concentrated in vacuo, the residue was diluted with water (200 ml) and extracted with ethyl acetate (200 ml). The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to give ethyl trans-5-(4-benzyloxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate (9.8 g) as needles (mp=130°-131° C.).

후처리

  1. concentrationAfter the mixture was concentrated in vacuo
  2. additionthe residue was diluted with water (200 ml)
  3. extractionextracted with ethyl acetate (200 ml)
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-0bc1a7edcd584f338aa5705126d111be
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05726306

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