Thionyl Chloride → 3-Chlorocarbonyl-10,11-dihydro-11-oxodibenzo[b,f]thiepin

반응식

[O:1]=[C:2]1[CH2:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[S:5][C:4]2[CH:13]=[C:14]([C:17]([OH:19])=O)[CH:15]=[CH:16][C:3]1=2.S(Cl)([Cl:22])=O>>[Cl:22][C:17]([C:14]1[CH:15]=[CH:16][C:3]2[C:2](=[O:1])[CH2:8][C:7]3[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=3[S:5][C:4]=2[CH:13]=1)=[O:19]

참가 물질

반응물 2

HCID 24386Thionyl Chloride

HCID 8270515-oxo-6H-benzo[b][1]benzothiepine-2-carboxylic acid

생성물 1

HCID 202702113-Chlorocarbonyl-10,11-dihydro-11-oxodibenzo[b,f]thiepin

실험 절차

Heat a solution of 5 g. of 10,11-dihydro-11-oxodibenzo[b,f]thiepin-3-carboxylic acid and 40 ml. of thionyl chloride under reflux for 20 minutes. Evaporate the reaction mixture under vacuum to dryness. Repeat the evaporation with two 30 ml. portions of carbon tetrachloride. Crystallize the residue from diisopropyl ether to obtain the title product.

후처리

temperatureHeat a solution of 5 g
customEvaporate the reaction mixture under vacuum to dryness
customRepeat the evaporation with two 30 ml
customCrystallize the residue from diisopropyl ether

출처 및 근거

ORD 기록: ord-2af09a19d91e4b68a46aad7a9be70990
출처 데이터셋: uspto-grants-1983_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04394515

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