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Diethyl Ether → 4-Methoxymethylbezyl 2,2-dimethyl-3-(3-methoxy-3-oxo-1-propenyl)cyclopropanecarboxylate

HRID 1872078
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HRID 1872078 반응식
[CH3:1][C:2]1([CH3:14])[CH:4]([CH:5]=[CH:6][C:7]([O:9][CH3:10])=[O:8])[CH:3]1[C:11]([OH:13])=[O:12].[CH3:15][O:16][CH2:17][C:18]1[CH:25]=[CH:24][C:21]([CH2:22]Br)=[CH:20][CH:19]=1.C(N(CC)CC)C.CCOCC>CC(C)=O>[CH3:1][C:2]1([CH3:14])[CH:4]([CH:5]=[CH:6][C:7]([O:9][CH3:10])=[O:8])[CH:3]1[C:11]([O:13][CH2:22][C:21]1[CH:24]=[CH:25][C:18]([CH2:17][O:16][CH3:15])=[CH:19][CH:20]=1)=[O:12]
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참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 8471TriethylamineHCID 112643741-(Bromomethyl)-4-(methoxymethyl)benzeneHCID 545573312,2-Dimethyl-3-(3-methoxy-3-oxo-1-propenyl) cyclopropanecarboxylic acid

생성물 1

HCID 543222844-Methoxymethylbezyl 2,2-dimethyl-3-(3-methoxy-3-oxo-1-propenyl)cyclopropanecarboxylate수율 94.8%

시약·촉매·용매 1

HCID 180
Acetone
용매

실험 절차

4.1 g of 2,2-dimethyl-3-(3-methoxy-3-oxo-1-propenyl) cyclopropanecarboxylic acid was dissolved in 50 ml of acetone, and 4.3 g of 4-methoxymethylbezylbromide was added to the solution. Next 2.4 g of triethylamine was added to the solution and underwent reaction at 60-80° C. for 3 hours while agitated, after which ether was added. After the ether solution was fully washed with diluted hydrochloric acid, sodium hydrogencarbonate aqueous solution and brine, it was dried with mirabilite. Ether was distilled under reduced pressure, and 6.3 g of 4-methoxymethylbezyl 2,2-dimethyl-3-(3-methoxy-3-oxo-1-propenyl)cyclopropanecarboxylate was obtained.

후처리

  1. washAfter the ether solution was fully washed with diluted hydrochloric acid, sodium hydrogencarbonate aqueous solution and brine, it
  2. dry with materialwas dried with mirabilite
  3. distillationEther was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-72fb62b8cf3a46dd966bdcb72b3dd6d3
출처 데이터셋
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06107339

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