Ethylene Glycol → N-(1-ethyl-2-pyrrolidyl-methyl)-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxamide

HRID 1413168노트

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HRID 1413168 반응식
CO[C:3]([C:5]1[C:14]2[O:13][CH2:12][CH2:11][O:10][C:9]=2[C:8]([O:15][CH3:16])=[C:7]([S:17](=[O:20])(=[O:19])[NH2:18])[CH:6]=1)=[O:4].C(O)CO.[CH2:25]([N:27]1[CH2:31][CH2:30][CH2:29][CH:28]1[CH2:32][NH2:33])[CH3:26].O>C(O)(=O)C>[CH2:25]([N:27]1[CH2:31][CH2:30][CH2:29][CH:28]1[CH2:32][NH:33][C:3]([C:5]1[C:14]2[O:13][CH2:12][CH2:11][O:10][C:9]=2[C:8]([O:15][CH3:16])=[C:7]([S:17](=[O:19])(=[O:20])[NH2:18])[CH:6]=1)=[O:4])[CH3:26]

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 962WaterHCID 1172952-Aminomethyl-1-ethylpyrrolidineHCID 20544706Methyl-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylate

생성물 1

HCID 20293649N-(1-ethyl-2-pyrrolidyl-methyl)-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxamide수율 73%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
50 °C

실험 절차

150 g of methyl-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylate and 750 cm3 of ethylene glycol were introduced into a balloon flask. After dissolution, 127 g of 1-ethyl-2-aminomethylpyrrolidine was added and the mixture was heated at 50° C. The resulting solution was dissolved with 2 liters of water and acidified by means of 120 cm3 of acetic acid. The precipitate formed was dried off, washed with water and then dried. The precipitate was then redissolved in 915 cm3 of hot water. The solution was filtered and then the base was precipitated with ammonia. The precipitate was dried off, washed with water and then dried. 144 g of N-(1-ethyl-2-pyrrolidyl-methyl)-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 110°-115° C.; yield: 73%).

후처리

  1. additionwas added
  2. customThe precipitate formed
  3. customwas dried off
  4. washwashed with water
  5. customdried
  6. dissolutionThe precipitate was then redissolved in 915 cm3 of hot water
  7. filtrationThe solution was filtered
  8. customthe base was precipitated with ammonia
  9. customThe precipitate was dried off
  10. washwashed with water
  11. customdried

출처 및 근거

ORD 기록
ord-00ee5519eb0e4358a6861214820e0cf5
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04248885

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