Potassium Carbonate → HCID 178515060、化合物

HRID 266435

反応式

HRID 266435 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 178515060HCID 178515060、化合物収率 81.7%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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+).

後処理

  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)

出典と根拠

ORDレコード
ord-8cbd179f41b64431aff323ddef88b0d0
出典データセット
uspto-grants-1997_07
特許番号
US05650422

関連ノート

読み込み中…