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

HRID 2395340

반응식

HRID 2395340 반응식
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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 119872-ChlorobenzothiazoleHCID 145104-Aminothiophenol

생성물 1

HCID 1176104-(2-Benzothiazol-2-ylthio)aniline수율 88.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-af3494c0b6ea4ff08fa12849fe1ef3a4
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05814646

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