Water → HCID 19787778, 화합물

반응식

[C:1]1([C:7]2[N:12]=[C:11]([CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:10](=O)[NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.P(Cl)(Cl)([Cl:24])=O>>[Cl:24][C:10]1[N:9]=[N:8][C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[N:12][C:11]=1[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

참가 물질

반응물 3

HCID 962Water

HCID 24813Phosphorus oxychloride

HCID 12358089HCID 12358089, 화합물

생성물 1

HCID 19787778HCID 19787778, 화합물

실험 절차

Heat a solution of 15 mmol (4 g) of 3-phenyl-5-benzyl-1,2,4-triazin-6-one obtained in Step C of Example 28 in 30 ml of phosphorus oxychloride to a temperature of 80° C. After cooling, pour into iced water, render alkaline and extract with ethyl acetate. Dry the organic phase, filter, evaporate to dryness and purify by chromatography on silica (eluant ethyl acetate/hexane: 27/75)

후처리

temperatureAfter cooling
extractionextract with ethyl acetate
customDry the organic phase
filtrationfilter
customevaporate to dryness
custompurify by chromatography on silica (eluant ethyl acetate/hexane: 27/75)

출처 및 근거

ORD 기록: ord-eedb14be5ffc41c09fa0ec12526ae4ac
출처 데이터셋: uspto-grants-1993_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05254548

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