2,4-Dichloro-6-methylquinoline → 4-(4-Chloro-6-methylquinolin-2-yl)-8-methoxy-2,3,4,5-tetrahydro-1,4-benzothiazepine

HRID 539993노트

반응식

HRID 539993 반응식
[CH3:1][O:2][C:3]1[CH:13]=[CH:12][C:6]2[CH2:7][NH:8][CH2:9][CH2:10][S:11][C:5]=2[CH:4]=1.Cl[C:15]1[CH:24]=[C:23]([Cl:25])[C:22]2[C:17](=[CH:18][CH:19]=[C:20]([CH3:26])[CH:21]=2)[N:16]=1>C(O)CCC>[Cl:25][C:23]1[C:22]2[C:17](=[CH:18][CH:19]=[C:20]([CH3:26])[CH:21]=2)[N:16]=[C:15]([N:8]2[CH2:7][C:6]3[CH:12]=[CH:13][C:3]([O:2][CH3:1])=[CH:4][C:5]=3[S:11][CH2:10][CH2:9]2)[CH:24]=1

참가 물질

4

반응물 2

HCID 27546682,4-Dichloro-6-methylquinolineHCID 857659308-Methoxy-2,3,4,5-tetrahydro-1,4-benzothiazepine

생성물 1

HCID 712555524-(4-Chloro-6-methylquinolin-2-yl)-8-methoxy-2,3,4,5-tetrahydro-1,4-benzothiazepine수율 50%

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
160 °C

실험 절차

A mixture of 8-methoxy-2,3,4,5-tetrahydro-1,4-benzothiazepine (0.63 g, 3.2 mmol), 2,4-dichloro-6-methylquinoline (0.68 g, 3.2 mmol) and n-butanol (4 mL) was heated with stirring in a 5 mL of microwave process vial for 2.5 hours at 160° C. under microwave irradiation. The solvent was removed by concentration in vacuo. The residue was dissolved in a mixture solvent of ethanol and dichloromethane and then concentrated in vacuo to remove dichloromethane. The formed precipitate was collected by filtration, which was washed with diethyl ether and petroleum ether, dried in vacuo to afford 0.59 g of the product as a pale white solid (yield was 50%). MS obsd. (ESI+) [(M+H)+] 371.

후처리

  1. temperaturewas heated
  2. customThe solvent was removed by concentration in vacuo
  3. dissolutionThe residue was dissolved in a mixture solvent of ethanol and dichloromethane
  4. concentrationconcentrated in vacuo
  5. customto remove dichloromethane
  6. filtrationThe formed precipitate was collected by filtration, which
  7. washwas washed with diethyl ether and petroleum ether
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-4e1218206b1b4e1eba2589a356cb2bdd
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871756B2

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