Ethyl formate → Ethyl 2-[(2H-1,3-benzodioxol-5-yl)methyl]-3-oxopropanoate

HRID 1445306노트

반응식

HRID 1445306 반응식
[H-].[Na+].[CH2:3]1[O:11][C:10]2[CH:9]=[CH:8][C:7]([CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:6][C:5]=2[O:4]1.[CH:19](OCC)=[O:20]>O1CCCC1>[CH:19]([CH:13]([CH2:12][C:7]1[CH:8]=[CH:9][C:10]2[O:11][CH2:3][O:4][C:5]=2[CH:6]=1)[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:20]

참가 물질

5

반응물 3

HCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 81545Ethyl 1,3-benzodioxole-5-propionate

생성물 1

HCID 10060648Ethyl 2-[(2H-1,3-benzodioxol-5-yl)methyl]-3-oxopropanoate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

First, 42.4 g of 60% NaH was suspended in 500 ml of tetrahydrofuran (THF). 84.5 g (purity: 93.7% by weight) of ethyl 3-(3,4-methylenedioxyphenyl)-propionate was dissolved in 100 ml of THF and added dropwise to the suspension solution prepared above at room temperature. After the resultant suspension solution was raised in temperature to 40° C. and stirred for 15 minutes, 131 g of ethyl formate was added dropwise for 2.5 hours to the suspension solution and stirred for a further 3 hours.

후처리

  1. additionadded dropwise to the suspension solution
  2. customprepared above at room temperature
  3. stirringstirred for a further 3 hours

출처 및 근거

ORD 기록
ord-98f38d7cc9aa4ea591aa80a17b083bf6
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07666659B2

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