2-Aminopyridine → 2-(chloromethyl)-4H-pyrido(1,2-a)pyrimidin-4-one

반응식

[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH2:7].[Cl:8][CH2:9][C:10](=O)[CH2:11][C:12](OCC)=[O:13]>>[Cl:8][CH2:9][C:10]1[N:7]=[C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][N:1]2[C:12](=[O:13])[CH:11]=1

참가 물질

반응물 2

HCID 104392-Aminopyridine

HCID 69484Ethyl 4-chloroacetoacetate

생성물 1

HCID 51550272-(chloromethyl)-4H-pyrido(1,2-a)pyrimidin-4-one

실험 절차

37.7 g 2-pyridinamine was dissolved in about 250 g polyphosphoric acid, at 40°-50°, using a mechanically driven stirrer. To this mixture was added, dropwise, 54 ml ethyl 4-chloroacetoacetate. After the addition, the mixture was heated to about 125° for 1/2 hour. After cooling to about 50°, the mixture was poured into 1500 ml of ice water, and the mixture was extracted with an equal volume of chloroform. After drying and evaporation of chloroform, about 45 g 2-(chloromethyl)-4H-pyrido[1,2-a] pyrimidin-4-one (m.p. 171°-174°) was obtained.

후처리

additionTo this mixture was added
additionAfter the addition
temperaturethe mixture was heated to about 125° for 1/2 hour
temperatureAfter cooling to about 50°
extractionthe mixture was extracted with an equal volume of chloroform
customAfter drying
customevaporation of chloroform

출처 및 근거

ORD 기록: ord-51d8c9f0269e46278fcd44d7fff2a781
출처 데이터셋: uspto-grants-1983_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04395551

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