Methanesulfonic Acid → 2-(4-Aminophenyl)benzothiazole methanesulphonic acid salt

HRID 363303

반응식

HRID 363303 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:4][CH:3]=1.[CH3:17][S:18]([OH:21])(=[O:20])=[O:19]>C(OCC)(=O)C>[CH3:17][S:18]([OH:21])(=[O:20])=[O:19].[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 2344752-(4-Aminophenyl)benzothiazole

생성물 1

HCID 877273232-(4-Aminophenyl)benzothiazole methanesulphonic acid salt수율 94%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-(4-aminophenyl)benzothiazole (0.5 g, 2.21 mmol) in ethyl acetate (65 ml) was added dropwise methanesulphonic acid (0.215 g, 2.21 mmol) at room temperature. The reaction mixture was stirred for 30 minutes. The product was collected and washed with hot ethyl acetate to give a pale yellow powder (0.67 g, 94%), m.p. 261°-262° C.; vmax /cm-1 3422, 2880, 2633, 1598, 1487, 1322, 1220, 1149, 1043, 967, 780, 755, 561; δH (DMSO-d6) 8.10(1H, d, J7.9, 4-H), 8.00(3H, m, 7, 2', 6'-H), 7.52(1H, t, J7.3, 5-H), 7.42(1H, t, J7.5, 6-H), 7.06(2H, d, J8.5, 3', 5'-H), 5.72(3H, br s, NH3+), 2.41(3H, s, CH3).

후처리

  1. customThe product was collected
  2. washwashed with hot ethyl acetate

출처 및 근거

ORD 기록
ord-5c0dc69af73046c59c49b435471033a0
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05874431

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