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

HRID 1872078
ノート
印刷プレビュー

反応式

HRID 1872078 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180
Acetone
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-72fb62b8cf3a46dd966bdcb72b3dd6d3
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06107339

反応ノート

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