Ethyl bromoacetate → Ethyl (1-oxo-2-ethyl-6,7-dichloro-5-indanyloxy)acetate

HRID 1834680노트

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HRID 1834680 반응식
[CH2:1]([CH:3]1[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[CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25]>CN(C)C=O>[O:15]=[C:4]1[C:5]2[C:10](=[CH:9][C:8]([O:12][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])=[C:7]([Cl:13])[C:6]=2[Cl:14])[CH2:11][CH:3]1[CH2:1][CH3:2]

참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 128572202-Ethyl-5-hydroxy-6,7-dichloroindanone

생성물 1

HCID 53855486Ethyl (1-oxo-2-ethyl-6,7-dichloro-5-indanyloxy)acetate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

A mixture of 2-ethyl-5-hydroxy-6,7-dichloro-1-indanone (9.8 g., 0.04 mole), dimethylformamide (30 ml.), potassium carbonate (12.5 g., 0.09 mole) and ethyl bromoacetate (15 g., 0.09 mole) is stirred and heated on a water bath at 60° C. for one hour. The reaction mixture is poured into ice water (200 ml.) and extracted with two 50 ml. portions of ether. The ether extract is washed with water, dried over magnesium sulfate and the ether distilled at reduced pressure. The ethyl (1-oxo-2-ethyl-6,7-dichloro-5-indanyloxy)acetate thus obtained melts at 116°-118° C. after recrystallization from ethyl alcohol.

후처리

  1. extractionextracted with two 50 ml
  2. extractionThe ether extract
  3. washis washed with water
  4. dry with materialdried over magnesium sulfate
  5. distillationthe ether distilled at reduced pressure
  6. customThe ethyl (1-oxo-2-ethyl-6,7-dichloro-5-indanyloxy)acetate thus obtained melts at 116°-118° C. after recrystallization from ethyl alcohol

출처 및 근거

ORD 기록
ord-de51f3168d194251b2214bc579280f51
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04070539

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