Hydrochloric Acid → HCID 67046796, 화합물

HRID 607511노트

반응식

HRID 607511 반응식
[CH3:1][C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[NH2:4].N1C=C[CH:12]=[CH:11][CH:10]=1.[CH3:15][S:16](Cl)(=[O:18])=[O:17].[Cl-].[Cl-].[Cl-].[Al+3].C(Cl)(=[O:26])C.Cl>C(Cl)Cl.C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:8]=[C:7]([C:10](=[O:26])[CH2:11][CH3:12])[CH:6]=[CH:5][C:3]=1[NH:4][S:16]([CH3:15])(=[O:18])=[O:17]

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6367Acetyl chlorideHCID 7242O-ToluidineHCID 31297Methanesulfonyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 67046796HCID 67046796, 화합물수율 43.5%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-methylaniline (2.2 g, 20 mmol, purchased from TCI) in pyridine (1.7 ml. 1.7 g, 21.4 mmol) and DCM (85 ml), methanesulfonyl chloride (1.6 ml, 2.3 g, 20 mmol) was added dropwise over 10 minutes at 0° C. The reaction mixture was stirred at room temperature for 1 hour. After cooling to 0° C., aluminum trichloride (6.8 g, 51 mmol) was added to the reaction mixture carefully. Then acetyl chloride (1.9 g, 20 mmol) was added dropwise over 15 minutes. The reaction mixture was diluted with toluene (25 ml) and poured into 2 M HCl aqueous solution (500 ml) with stirring at 0° C. The precipitates were filtered, washed with water and dried in vacuo to afford the title compound (2.1 g, 43%) as yellow solids.

후처리

  1. temperatureAfter cooling to 0° C.
  2. stirringwith stirring at 0° C
  3. filtrationThe precipitates were filtered
  4. washwashed with water
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-ce0fe23490154856964ab4c233aba79c
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915448B2

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