Dichloromethane → 2-(2-Methoxy-4-nitrophenyl)benzothiazole

HRID 339495

반응식

HRID 339495 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[SH:8].[CH3:9][O:10][C:11]1[CH:19]=[C:18]([N+:20]([O-:22])=[O:21])[CH:17]=[CH:16][C:12]=1[C:13](O)=O.C(Cl)Cl>CCOCC>[CH3:9][O:10][C:11]1[CH:19]=[C:18]([N+:20]([O-:22])=[O:21])[CH:17]=[CH:16][C:12]=1[C:13]1[S:8][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[N:1]=1

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 87132-AminothiophenolHCID 757764-Nitro-o-anisic acid

생성물 1

HCID 672372802-(2-Methoxy-4-nitrophenyl)benzothiazole수율 62%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
150 °C

실험 절차

A thoroughly mixed paste of 2-aminobenzenethiol (0.63 g, 5.07 mmol) and 2-methoxy-4-nitrobenzoic acid (1.0 g, 5.07 mmol) in trimethylsilylpolyphosphate (5 ml) was stirred and heated at 150° C. under an atmosphere of argon for 1.5 h. On cooling to room temperature the reaction mixture was a solid mass to which was added DCM (35 ml) and Et2O (50 ml). The solid was broken up and collected by filtration, then recrystallised from AcOH and dried under high vacuum for 18 h to give the title compound (0.90 g, 62%) as a yellow solid.

후처리

  1. temperatureOn cooling to room temperature the reaction mixture
  2. filtrationcollected by filtration
  3. customrecrystallised from AcOH
  4. customdried under high vacuum for 18 h

출처 및 근거

ORD 기록
ord-a24f807588bb43c18473164e23930830
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895313B2

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