Potassium Carbonate → HCID 178515060, 화합물

HRID 266435노트

반응식

HRID 266435 반응식
Cl[CH2:2][N:3]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[S:4]1(=[O:6])=[O:5].C1([N:21]2[C:25]([SH:26])=[N:24][N:23]=[N:22]2)CCCCC1.C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C>[CH:7]1([CH:2]([S:26][C:25]2[NH:24][N:23]=[N:22][N:21]=2)[N:3]2[C:13](=[O:14])[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:4]2(=[O:6])=[O:5])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 23024352-(Chloromethyl)-2,3-dihydro-1lambda6,2-benzothiazole-1,1,3-trioneHCID 178527987HCID 178527987, 화합물

생성물 1

HCID 178515060HCID 178515060, 화합물수율 81.7%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A mixture of 2-(chloromethyl) saccharin (3 g, 12.9 mmol) , 1-cyclohexyl-5-mercapto-1H-tetrazole (2.37 g, 12.9 mmol) and potassium carbonate (4.45 g, 32.2 mmol) was heated under reflux in methyl ethyl ketone (50 ml) for 1 hour. The reaction mixture was cooled, poured into dilute sodium bicarbonate/ice solution and extracted twice with ethyl acetate. The combined organic extracts were washed with water, dried (Na2SO4) and freed of solvent under vacuum. Chromatography (silica gel; MDC) afforded 2 g of 2-(1-cyclohexyl-1H-tetrazol-5-ylthiomethyl) saccharin as a white foam that was crystallized from hot cyclohexane, mp 103°-105° C. 1H nmr (90 MHz, CDCl3):5.65 (2H, s). FDMS: m/e 379 (M+).

후처리

  1. temperaturewas heated
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted twice with ethyl acetate
  4. washThe combined organic extracts were washed with water
  5. dry with materialdried (Na2SO4)

출처 및 근거

ORD 기록
ord-8cbd179f41b64431aff323ddef88b0d0
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05650422

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