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

HRID 1679714노트

반응식

HRID 1679714 반응식
[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]

참가 물질

7

반응물 4

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 12395586HCID 12395586, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매2회HCID 6228Dimethylformamide용매

반응 조건

온도
55 °C

실험 절차

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 1 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.

후처리

  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

출처 및 근거

ORD 기록
ord-e651aed7cb6c4194a72b27cd3e2132ad
출처 데이터셋
uspto-grants-1978_03
특허 번호
US04081554

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