Acetone → HCID 131711713, 화합물

HRID 1660038노트

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HRID 1660038 반응식
[CH:1]1([NH:7][S:8]([C:11]2[CH:12]=[C:13]([C:21]([OH:23])=O)[C:14]3[O:19][CH2:18][CH2:17][O:16][C:15]=3[CH:20]=2)(=[O:10])=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.O.ClC(OC[CH:30]([CH3:32])C)=O.C([NH:35]CC)C.C[C:39]([CH3:41])=O>C(N(CC)CC)C>[CH2:39]([C:20]1[C:15]2[O:16][CH2:17][CH2:18][O:19][C:14]=2[C:13]([C:21]([NH2:35])=[O:23])=[C:12]([CH2:30][CH3:32])[C:11]=1[S:8](=[O:9])(=[O:10])[NH:7][CH:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1)[CH3:41]

참가 물질

7

반응물 5

HCID 180AcetoneHCID 962WaterHCID 8021DiethylamineHCID 62365Isobutyl chloroformateHCID 205447497-Cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxylic acid

생성물 1

HCID 131711713HCID 131711713, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

반응 조건

온도
10 °C

실험 절차

34.1 g of 7-cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxylic acid, 35 ml of water and 10.5 g of triethylamine were introduced into a 250 ml balloon flask provided with a stirrer and a thermometer. 100 ml of acetone were added and the mixture was cooled to 10° C. 14 g of isobutyl chloroformate were added and the mixture was maintained under stirring for 30 minutes at room temperature. 8 g of diethylamine were introduced at a temperature of from 15°-20° C. After stirring for three hours, the solvent was removed under vacuum. The residue was washed with water, dried, dissolved in 180 ml of absolute ethanol and treated with 3 g of black carbon. After filtration and crystallization, 23 g of diethyl-7-cyclohexylsulfamoyl-1,4-benzodioxane-5-carboxamide were obtained (M.P.: 201° C.). The structure was confirmed by infrared and nuclear magnetic resonance analyses.

후처리

  1. customprovided with a stirrer
  2. temperaturethe mixture was maintained
  3. stirringAfter stirring for three hours
  4. customthe solvent was removed under vacuum
  5. washThe residue was washed with water
  6. customdried
  7. dissolutiondissolved in 180 ml of absolute ethanol
  8. additiontreated with 3 g of black carbon
  9. filtrationAfter filtration and crystallization

출처 및 근거

ORD 기록
ord-28eb3def46f349a7887845fd68ca24f8
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04306072

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