Potassium Carbonate → 4-(2-Benzothiazol-2-ylthio)aniline

HRID 55084

反応式

HRID 55084 の反応式
Cl[C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[NH2:11][C:12]1[CH:17]=[CH:16][C:15]([SH:18])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[NH2:11][C:12]1[CH:17]=[CH:16][C:15]([S:18][C:2]2[S:3][C:4]3[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=3[N:6]=2)=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 119872-ChlorobenzothiazoleHCID 145104-Aminothiophenol

生成物 1

HCID 1176104-(2-Benzothiazol-2-ylthio)aniline収率 88.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Chlorobenzothiazole (0.06 moles, 10.1 g), 4-aminothiophenol (0.06 moles, 7.5 g) and potassium carbonate (0.06 moles, 8.3 g) were stirred for 3 days at room temperature in 250 ml ethanol, filtered, and concentrated. Ethyl acetate was added and the solution washed with water, dried over sodium sulfate and concentrated. The product was purified by HPLC over silica gel eluted with 40-60% ethyl acetate in hexane to yield 2-(4-aminophenylthio)benzothiazole 13.7 g, 88%. Mass spec (FD) 258. Calculated for C11H10N2S2:C, 60.44; H, 3.90; N, 10.84. Found: C, 60.63; H, 3.98; N, 11.01.

後処理

  1. filtrationfiltered
  2. concentrationconcentrated
  3. additionEthyl acetate was added
  4. washthe solution washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe product was purified by HPLC over silica gel
  8. washeluted with 40-60% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-d19d97a641a448f4938338c0b9f8cf75
出典データセット
uspto-grants-1997_04
特許番号
US05624937

関連ノート

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