Hexane → 2-Methyl-6-(piperidine-1-sulfonyl)-benzothiazole

HRID 84775

반응식

HRID 84775 반응식
[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[C:9]([S:11](Cl)(=[O:13])=[O:12])[CH:8]=[CH:7][C:5]=2[N:6]=1.[NH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1.CCCCCC>C(Cl)(Cl)Cl.C(OCC)(=O)C>[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[C:9]([S:11]([N:15]3[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]3)(=[O:13])=[O:12])[CH:8]=[CH:7][C:5]=2[N:6]=1

참가 물질

6

반응물 3

HCID 8058HexaneHCID 8082PiperidineHCID 35830192-Methyl-1,3-benzothiazole-6-sulfonyl chloride

생성물 1

HCID 10756752-Methyl-6-(piperidine-1-sulfonyl)-benzothiazole수율 74.2%

시약·촉매·용매 2

HCID 6212Chloroform용매2회HCID 8857Ethyl Acetate용매

실험 절차

A solution of Compound 2 (2.5 g, 10 mmol) in chloroform (15 ml) was added drop wise to a solution of piperidine (1.7 g, 20.0 mmol) in chloroform (10 ml). The combined mixture was stirred at room temperature for 1 hour. The reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml). The organic layer was dried with sodium sulfate and evaporated. The sticky white solid thus obtained was dissolved in ca. 5 ml of hot ethyl acetate and this solution was then slowly added to 40 ml hexane. The white solid that precipitated was collected, washed with hexane and dried to yield 2.2 g (74%) of Compound 3, Rf=0.28 (30% ethyl acetate in hexane). The structure of Compound 3 is given below:

후처리

  1. washThe reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml)
  2. dry with materialThe organic layer was dried with sodium sulfate
  3. customevaporated
  4. customThe sticky white solid thus obtained
  5. customThe white solid that precipitated
  6. customwas collected
  7. washwashed with hexane
  8. customdried

출처 및 근거

ORD 기록
ord-bfeb1d4046c14d1f9bb293b538594a73
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846952B2

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