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Ethyl bromoacetate → Ethyl {[6-cyano-6-(4-methoxydibenzo[b,d]furan-1-yl)-2-methyl-5,6,7,8-tetrahydro quinazolin-4-yl]oxy}acetate

HRID 2383989
ノート
印刷プレビュー

反応式

HRID 2383989 の反応式
[CH3:1][O:2][C:3]1[C:8]2[O:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[C:7]=2[C:6]([C:16]2([C:28]#[N:29])[CH2:25][CH2:24][C:23]3[N:22]=[C:21]([CH3:26])[NH:20][C:19](=[O:27])[C:18]=3[CH2:17]2)=[CH:5][CH:4]=1.[CH2:30]([O:32][C:33](=[O:36])[CH2:34]Br)[CH3:31].C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.O>[C:28]([C:16]1([C:6]2[C:7]3[C:11]4[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=4[O:9][C:8]=3[C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[CH2:25][CH2:24][C:23]2[N:22]=[C:21]([CH3:26])[N:20]=[C:19]([O:27][CH2:34][C:33]([O:32][CH2:30][CH3:31])=[O:36])[C:18]=2[CH2:17]1)#[N:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7748Ethyl bromoacetateHCID 10796Cesium carbonateHCID 1356204916-(4-Methoxydibenzo[b,d]furan-1-yl)-2-methyl-4-oxo-3,4,5,6,7,8-hexahydroquinazoline-6-carbonitrile

生成物 1

HCID 24804611Ethyl {[6-cyano-6-(4-methoxydibenzo[b,d]furan-1-yl)-2-methyl-5,6,7,8-tetrahydro quinazolin-4-yl]oxy}acetate

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

実験手順

To a solution of the compound obtained in example 21 (150 mg, 1.76 mmles) in dry DMF (5 ml) was added ethylbromoacetate (322.3 mg, 1.93 mmol) and cesium carbonate (688 mg, 2.11 mmol). The reaction mass was stirred at room temperature for 1 hr, diluted with water and extracted with ethyl acetate. The organic layer was washed with water followed by brine and dried over sodium sulfate and concentrated under vacuum. The crude product was purified by column chromatography to get both pure compounds.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under vacuum
  5. customThe crude product was purified by column chromatography
  6. customto get both pure compounds

出典と根拠

ORDレコード
ord-9059a38c5f844c03b8cf23c6b9fb767b
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08263648B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート