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

HRID 363303

反応式

HRID 363303 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-5c0dc69af73046c59c49b435471033a0
出典データセット
uspto-grants-1999_02
特許番号
US05874431

関連ノート

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