Sodium Carbonate → HCID 15296730、化合物

HRID 2226902

反応式

HRID 2226902 の反応式
[C:1]1([CH:7]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:8]([N:10]2[CH:19]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:18][C:17]3[C:12](=[CH:13][CH:14]=[C:15]([O:26][CH3:27])[C:16]=3[OH:25])[CH2:11]2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:34]([C:38]1[CH:45]=[CH:44][C:41]([CH2:42]Br)=[CH:40][CH:39]=1)([O:36][CH3:37])=[O:35].C(=O)([O-])[O-].[Na+].[Na+]>CN(C=O)C>[C:34]([C:38]1[CH:45]=[CH:44][C:41]([CH2:42][O:25][C:16]2[C:15]([O:26][CH3:27])=[CH:14][CH:13]=[C:12]3[C:17]=2[CH2:18][CH:19]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[N:10]([C:8](=[O:9])[CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)[CH2:11]3)=[CH:40][CH:39]=1)([O:36][CH3:37])=[O:35]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 256687Methyl 4-(bromomethyl)benzoateHCID 15296729(RS)-2-(Diphenylacetyl)-1,2,3,4-tetrahydro-5-hydroxy-6-methoxy-3-isoquinolinecarboxylic acid, ethyl ester

生成物 1

HCID 15296730HCID 15296730、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 0.89 g (0.002 mole) of the compound from Example 31, 0.69 g (0.003 mole) of 4-carbomethoxybenzyl bromide (Aldrich), 5.0 g of powdered anhydrous sodium carbonate, and 5 mL of DMF is heated at reflux, with stirring, for 5 minutes. The cooled mixture is treated with 50 mL of ice water. The precipitated product is extracted into 150 mL of ether. The solution is dried (magnesium sulfate) and concentrated; wt. of amorphous solid 1.20 g; mass spectrum (CI) 594 (M+).

後処理

  1. temperatureis heated
  2. temperatureat reflux
  3. extractionThe precipitated product is extracted into 150 mL of ether
  4. dry with materialThe solution is dried (magnesium sulfate)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-66f4044cba9f422da08c2717ef8e966c
出典データセット
uspto-grants-1994_09
特許番号
US05350757

関連ノート

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