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Potassium Carbonate → HCID 67604482、化合物

HRID 1419065
ノート
印刷プレビュー

反応式

HRID 1419065 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 67604482HCID 67604482、化合物収率 81.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.).

後処理

  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)

出典と根拠

ORDレコード
ord-39f258afb60649b586bb0c16776ca3f5
出典データセット
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05885979

反応ノート

読み込み中…

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