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Pyridine → Ethyl-3-Chloromethyl-4-oxo-3-H-phthalazin-1-ylacetate

HRID 1199502
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인쇄 미리보기

반응식

HRID 1199502 반응식
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9](=[O:16])[N:8]([CH2:17]O)[N:7]=1)[CH3:2].CS([Cl:24])(=O)=O.N1C=CC=CC=1>C(Cl)Cl>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9](=[O:16])[N:8]([CH2:17][Cl:24])[N:7]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 14519538HCID 14519538, 화합물

생성물 1

HCID 14519542Ethyl-3-Chloromethyl-4-oxo-3-H-phthalazin-1-ylacetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of ethyl-3-hydroxymethyl-4-oxo-3-H-phthalazin-1-ylacetate (1.31 g) and methanesulfonyl chloride (0.69 g) in methylene chloride (10 ml) containing pyridine (0.8 ml) was stirred at room temperature overnight. Upon evaporation of methylene chloride and purification of the residue by chromatography on silica gel, eluting with a mixture of a chloroform and ethyl acetate (9:1), the title product was obtained (yield: 0.51 g; m.p. 99°-100° C.).

후처리

  1. customUpon evaporation of methylene chloride and purification of the residue by chromatography on silica gel
  2. washeluting with a mixture of a chloroform and ethyl acetate (9:1)

출처 및 근거

ORD 기록
ord-a0308490186840cc9a2f7a39fbe150d3
출처 데이터셋
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04900844

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