Ethyl bromoacetate → {[6,7-Dichloro-2-methyl-1-oxo-2-(propan-2-yl)-2,3-dihydro-1H-inden-5-yl]oxy}acetic acid

HRID 1287440ノート

反応式

HRID 1287440 の反応式
[CH3:1][C:2]1([CH:15]([CH3:17])[CH3:16])[CH2:10][C:9]2[C:4](=[C:5]([Cl:13])[C:6]([Cl:12])=[C:7]([OH:11])[CH:8]=2)[C:3]1=[O:14].C(=O)([O-])[O-].[K+].[K+].Br[CH2:25][C:26]([O:28]CC)=[O:27].[OH-].[Na+]>CN(C=O)C.O>[O:14]=[C:3]1[C:4]2[C:9](=[CH:8][C:7]([O:11][CH2:25][C:26]([OH:28])=[O:27])=[C:6]([Cl:12])[C:5]=2[Cl:13])[CH2:10][C:2]1([CH3:1])[CH:15]([CH3:17])[CH3:16]

参加物

7

反応物 4

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 12395586HCID 12395586、化合物

生成物 1

HCID 41029{[6,7-Dichloro-2-methyl-1-oxo-2-(propan-2-yl)-2,3-dihydro-1H-inden-5-yl]oxy}acetic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6228Dimethylformamide溶媒

反応条件

温度
55 °C

実験手順

A stirred mixture of 2-methyl-2-isopropyl-5-hydroxy-6,7-dichloro-1-indanone (6.2 g., 0.023 mole), potassium carbonate (7.3 g.), ethyl bromoacetate (8.5 g.) in DMF (70 ml.) is warmed in an inert atmosphere at 55° C. for one hour, then treated with water (60 ml.) and 10N sodium hydroxide (10 ml.) and heated on a steam bath for 1.5 hours. The reaction mixture is poured into water, acidified, extracted with ether, washed with water and dried over magnesium sulfate. Following evaporation of the ether there is obtained 5.1 g. of (1-oxo-2-methyl-2-isopropyl-6,7-dichloro-5-indanyloxy) acetic acid which melts at 156°-157°C. after recrystallization from nitromethane.

後処理

  1. temperatureheated on a steam bath for 1.5 hours
  2. extractionextracted with ether
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporation of the ether
  6. customthere is obtained 5.1 g
  7. customof (1-oxo-2-methyl-2-isopropyl-6,7-dichloro-5-indanyloxy) acetic acid which melts at 156°-157°C. after recrystallization from nitromethane

出典と根拠

ORDレコード
ord-a6e0786b18394b4d91cdc2e7f0ac0c26
出典データセット
uspto-grants-1976_10
特許番号
US03984465

反応ノート

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