Pyridine → 5-Chloro-thiophene-2-sulfonic acid (3-methyl-bicyclo[3.2.1]oct-8-yl)-amide

HRID 902439

반응식

HRID 902439 반응식
[CH3:1][CH:2]1[CH2:8][CH:7]2[CH:9]([NH2:10])[CH:4]([CH2:5][CH2:6]2)[CH2:3]1.[Cl:11][C:12]1[S:16][C:15]([S:17](Cl)(=[O:19])=[O:18])=[CH:14][CH:13]=1.N1C=CC=CC=1>C(Cl)Cl>[CH3:1][CH:2]1[CH2:3][CH:4]2[CH:9]([NH:10][S:17]([C:15]3[S:16][C:12]([Cl:11])=[CH:13][CH:14]=3)(=[O:19])=[O:18])[CH:7]([CH2:6][CH2:5]2)[CH2:8]1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 27339255-Chlorothiophene-2-sulfonyl chlorideHCID 179860493-Methyl-bicyclo[3.2.1]oct-8-ylamine

생성물 1

HCID 597018835-Chloro-thiophene-2-sulfonic acid (3-methyl-bicyclo[3.2.1]oct-8-yl)-amide수율 10%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-Methyl-bicyclo[3.2.1]oct-8-ylamine (prepared in Step 2, 0.165 mmol) was dissolved in DCM (1.5 mL) and treated with 5-chlorothiophenesulphonyl chloride (53.7 mg, 0.248 mmol) followed by pyridine (100 μL). The reaction was stirred at room temperature for 66 h, followed by heating at 60° C. for 18 h. The reaction mixture was evaporated and purified by mass-directed preparative HPLC to give the desired product (5.3 mg, 10%) as a mixture of four isomers. m/z 320 (M+H+).

후처리

  1. temperatureby heating at 60° C. for 18 h
  2. customThe reaction mixture was evaporated
  3. custompurified by mass-directed preparative HPLC

출처 및 근거

ORD 기록
ord-f426eb8f5f864e4fa84cba3b80e03055
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07365196B2

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