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Chlorosuccinimide → Ethyl 8-amino-7-chloro-2,3-dihydro-1,4-benzodioxine-5-carboxylate

HRID 1067274
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인쇄 미리보기

반응식

HRID 1067274 반응식
[NH2:1][C:2]1[C:7]2[O:8][CH2:9][CH2:10][O:11][C:6]=2[C:5]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:4][CH:3]=1.[Cl:17]N1C(=O)CCC1=O>O1CCOCC1.O>[NH2:1][C:2]1[C:7]2[O:8][CH2:9][CH2:10][O:11][C:6]=2[C:5]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:4][C:3]=1[Cl:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 31398ChlorosuccinimideHCID 15817382Ethyl 8-amino-2,3-dihydrobenzo[1,4]dioxine-5-carboxylate

생성물 1

HCID 15817383Ethyl 8-amino-7-chloro-2,3-dihydro-1,4-benzodioxine-5-carboxylate수율 98.8%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

37 g (0.165 mol) of ethyl 8-amino-2,3-dihydro-1,4-benzodioxine-5-carboxylate dissolved in 370 ml of dioxane are introduced into a 1 l round-bottomed flask, 23.2 g (0.174 mol) of N-chlorosuccinimide are added, at room temperature and with magnetic stirring, and the mixture is stirred overnight. It is diluted with water, extracted with ethyl acetate and, after the usual processing of the organic phase, 42 g of compound are obtained, which product is recrystallized from a mixture of diethyl ether and diisopropyl ether.

후처리

  1. additionare introduced into a 1 l round-bottomed flask
  2. extractionextracted with ethyl acetate

출처 및 근거

ORD 기록
ord-b0bd0cfe4d194ca19f4473507599a689
출처 데이터셋
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06248757B1

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