4-Aminothiophenol → HCID 18971644, 화합물

HRID 55086노트

반응식

HRID 55086 반응식
Cl[C:2]1[S:3][C:4]2[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:5]=2[N:6]=1.[NH2:12][C:13]1[CH:18]=[CH:17][C:16]([SH:19])=[CH:15][CH:14]=1>CN(C1C=CN=CC=1)C.C(O)C>[NH2:12][C:13]1[CH:18]=[CH:17][C:16]([S:19][C:2]2[S:3][C:4]3[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:5]=3[N:6]=2)=[CH:15][CH:14]=1

참가 물질

5

반응물 2

HCID 145104-AminothiophenolHCID 133148162,5-Dichloro-1,3-benzothiazole

생성물 1

HCID 18971644HCID 18971644, 화합물수율 22.3%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 702Ethanol용매

실험 절차

2,5-Dichlorobenzothiazole (0.049 moles, 10.0 g), 4-aminothiophenol (0.049 moles, 6.1 g) and DMAP (0.049 moles, 6.0 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 25% ethyl acetate in hexane to yield 2-(4-aminophenylthio)-5-chlorobenzothiazole 3.2 g, 22%. Mass spec (FD) 292. Calculated for C13H9ClN2S2 : C, 53.33; H, 3.10; N, 9.57. Found: C, 53.03; H, 3.30; N, 9.70.

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 25% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-1649a1ff85014499b6bc5f0bbaec4e76
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624937

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