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Hydrochloric Acid → Acetic acid, 6,7-dichloro-2-ethyl-2-methyl-1-oxo-5-indanyloxy-

HRID 2083445
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HRID 2083445 반응식
[CH2:1]([C:3]1([CH3:16])[CH2:11][C:10]2[C:5](=[C:6]([Cl:14])[C:7]([Cl:13])=[C:8]([OH:12])[CH:9]=2)[C:4]1=[O:15])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:24][C:25]([O:27]CC)=[O:26].[OH-].[Na+].Cl>CN(C=O)C.O>[O:15]=[C:4]1[C:5]2[C:10](=[CH:9][C:8]([O:12][CH2:24][C:25]([OH:27])=[O:26])=[C:7]([Cl:13])[C:6]=2[Cl:14])[CH2:11][C:3]1([CH2:1][CH3:2])[CH3:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 12395584HCID 12395584, 화합물

생성물 1

HCID 41028Acetic acid, 6,7-dichloro-2-ethyl-2-methyl-1-oxo-5-indanyloxy-

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

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온도
55 °C

실험 절차

A stirred mixture of 2-ethyl-2-methyl-5-hydroxy-6,7-dichloro-1-indanone (3.6 g., 0.014 mole), potassium carbonate (4.2 g.), ethyl bromoacetate (5.0 g.) in DMF (40 ml.) is warmed in an inert atmosphere at 55° C. for one hour, then treated with water (40 ml.) and 10N sodium hydroxide (6 ml.) and heated on a steam bath for 11/2 hours. The reaction mixture is poured into dilute aqueous hydrochloric acid, extracted with ether, washed with water and dried over magnesium sulfate. The ether is evaporated at reduced pressure affording the crude product which melts at 168° C. after recrystallization from nitromethane.

후처리

  1. temperatureheated on a steam bath for 11/2 hours
  2. extractionextracted with ether
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. customThe ether is evaporated at reduced pressure

출처 및 근거

ORD 기록
ord-79f6ea3fd92b4ea7a009ec246be372fc
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04085219

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