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Methanol → Methyl (1-oxo-2-ethyl-2,6,7-trichloro-5-indanyloxy)acetate

HRID 1834679
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HRID 1834679 반응식
[Cl-:1].[Li+].[O:3]=[C:4]1[C:12]2[C:7](=[CH:8][C:9]([O:15][CH2:16][C:17]([O:19][CH3:20])=[O:18])=[C:10]([Cl:14])[C:11]=2[Cl:13])[CH2:6][CH:5]1[CH2:21][CH3:22].CO>CN(C)C=O>[O:3]=[C:4]1[C:12]2[C:7](=[CH:8][C:9]([O:15][CH2:16][C:17]([O:19][CH3:20])=[O:18])=[C:10]([Cl:14])[C:11]=2[Cl:13])[CH2:6][C:5]1([CH2:21][CH3:22])[Cl:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 433294Lithium ChlorideHCID 13613301Methyl (1-oxo-2-ethyl-6,7-dichloro-5-indanyloxy)acetate

생성물 1

HCID 54266477Methyl (1-oxo-2-ethyl-2,6,7-trichloro-5-indanyloxy)acetate수율 53%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
90 °C

실험 절차

A stirred solution of cupric chloride dihydrate (4.25 g. and lithium chloride (0.765 g.) in dimethylformamide (10 ml.) is heated to 90° C. and to the mixture is added a solution of methyl (1-oxo-2-ethyl-6,7-dichloro-5-indanyloxy)-acetate (4.7 g., 0.015 mole) in dimethylformamide. The reaction mixture is heated at 90° C. for two hours and poured onto ice. The product is extracted into ether (100 ml.), washed with water, dried over anhydrous sodium sulfate and the ether distilled at reduced pressure. There is thus obtained 2.5 g. of methyl (1-oxo-2-ethyl-2,6,7-trichloro-5-indanyloxy)acetate (53% yield) which melts at 111° C. after recrystallization from methanol.

후처리

  1. additionpoured onto ice
  2. extractionThe product is extracted into ether (100 ml.)
  3. washwashed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe ether distilled at reduced pressure

출처 및 근거

ORD 기록
ord-7112deea57d4481786a1666c9d2e820d
출처 데이터셋
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04070539

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