1-Methylpyrrolidine-2-methylamine → N-(1-methyl-2-pyrrolidylmethyl)-1,4-benzodioxane-5-carboxamide

HRID 2285469ノート

反応式

HRID 2285469 の反応式
CO[C:3]([C:5]1[C:14]2[O:13][CH2:12][CH2:11][O:10][C:9]=2[CH:8]=[C:7](S(=O)(=O)NC)[CH:6]=1)=[O:4].[CH3:20][N:21]1[CH2:25][CH2:24][CH2:23][CH:22]1[CH2:26][NH2:27]>C(O)(=O)C.O>[CH3:20][N:21]1[CH2:25][CH2:24][CH2:23][CH:22]1[CH2:26][NH:27][C:3]([C:5]1[C:14]2[O:13][CH2:12][CH2:11][O:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)=[O:4]

参加物

5

反応物 2

HCID 1173001-Methylpyrrolidine-2-methylamineHCID 54343297Methyl-7-methylsulfamoyl-1,4-benzodioxane-5-carboxylate

生成物 1

HCID 53775438N-(1-methyl-2-pyrrolidylmethyl)-1,4-benzodioxane-5-carboxamide収率 112%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

実験手順

169 g of methyl-7-methylsulfamoyl-1,4-benzodioxane-5-carboxylate, 53 ml of water and 81 g of 1-methyl-2-aminomethylpyrrolidine were introduced into a balloon flask provided with a reflux condenser. The mixture was heated on a water bath until a test sample was totally soluble in dilute acids. The resulting crystals were dissolved in a solution of 50 ml of acetic acid in 1,250 ml of water and then the solution was filtered over carbon black and the base was reprecipitated by the addition of 100 ml of 20% ammonia. The crystals were dried off, washed with water and dried. 182 g of N-(1-methyl-2-pyrrolidylmethyl)-1,4-benzodioxane-5-carboxamide was produced (M.P.: 189°-190° C.; yield: 83.6%).

後処理

  1. customprovided with a reflux condenser
  2. temperatureThe mixture was heated on a water bath until a test sample
  3. filtrationthe solution was filtered over carbon black
  4. customthe base was reprecipitated by the addition of 100 ml of 20% ammonia
  5. customThe crystals were dried off
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-d2ee8c4916cf49c68de6be54276f9a19
出典データセット
uspto-grants-1982_04
特許番号
US04323503

反応ノート

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