Phosphorus oxychloride → 4-Chloro-6-iodo-2-(trifluoromethyl)quinazoline

반응식

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

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 135990571HCID 135990571, 화합물

생성물 1

HCID 190749504-Chloro-6-iodo-2-(trifluoromethyl)quinazoline

실험 절차

6-iodo-2-trifluoromethyl-3H-quinazolin-4-one (3.1 g, 9.1 mmole) was mixed with 20 mL of POCl3, heated to reflux for 3 h, removed most of unreacted POCl3 under vacuo. The residue was extracted with 15 mL of NaHCO3 (sat) and 200 mL of ether, ether layer was dried with MgSO4 and concentrated to give the light yellow solid 3.05 g, mp 145°-146° C., MS (CI): m/z 359 (MH)+.

후처리

temperatureheated
temperatureto reflux for 3 h
customremoved most of unreacted POCl3 under vacuo
extractionThe residue was extracted with 15 mL of NaHCO3 (sat) and 200 mL of ether, ether layer
dry with materialwas dried with MgSO4
concentrationconcentrated

출처 및 근거

ORD 기록: ord-1c2c0e41765540e09c1d2ad3da6ceec5
출처 데이터셋: uspto-grants-1997_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05658902

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