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Cyclopropylamine → HCID 53733396、化合物

HRID 652755
ノート
印刷プレビュー

反応式

HRID 652755 の反応式
Cl[CH:2]([CH2:19][CH2:20][CH2:21]Cl)[CH2:3][NH:4][C:5](=[O:18])[C:6]1[CH:11]=[C:10]([S:12](=[O:15])(=[O:14])[NH2:13])[CH:9]=[CH:8][C:7]=1[O:16][CH3:17].[CH:23]1([NH2:26])[CH2:25][CH2:24]1>O>[CH:23]1([N:26]2[CH2:21][CH2:20][CH2:19][CH:2]2[CH2:3][NH:4][C:5](=[O:18])[C:6]2[CH:11]=[C:10]([S:12](=[O:15])(=[O:14])[NH2:13])[CH:9]=[CH:8][C:7]=2[O:16][CH3:17])[CH2:25][CH2:24]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 69828CyclopropylamineHCID 30177965-(Aminosulphonyl)-N-(2,5-dichloropentyl)-2-methoxybenzamide

生成物 1

HCID 53733396HCID 53733396、化合物収率 189.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

36.9 g (0.1 mole) of N-(2,5-dichloropentyl)-2-methoxy-5-sulphamoyl-benzamide and 57 g of cyclopropylamine are placed in 250 ml bottle. They are brought to reflux for 6 hours, left to stand for 1 night then brought back to reflux for 5 hours. The suspension obtained is poured into 300 ml of water and 50 g of ice. The white precipitate is washed with water and dried in an oven at 60° C. It melts at 163° C. and weighs 29.5 g (83.6%). It is dissolved in 2 liters of acetonitrile and filtered in the presence of carbon black. The filtrate is left to crystallise. The crystals obtained are filtered, washed with acetonitrile and dried at 40° C. 67 g (yield 74.9%) of N-(1-cyclopropyl-2-pyrrolidinylmethyl)-2-methoxy-5-sulphamoylbenzamide is collected, melting at 180° C.

後処理

  1. temperatureto reflux for 6 hours
  2. waitleft
  3. waitto stand for 1 night
  4. temperatureto reflux for 5 hours
  5. customThe suspension obtained
  6. washThe white precipitate is washed with water
  7. customdried in an oven at 60° C
  8. dissolutionIt is dissolved in 2 liters of acetonitrile
  9. filtrationfiltered in the presence of carbon black
  10. waitThe filtrate is left
  11. customto crystallise
  12. customThe crystals obtained
  13. filtrationare filtered
  14. washwashed with acetonitrile
  15. customdried at 40° C

出典と根拠

ORDレコード
ord-47a372a3f332498995b12b5025af0244
出典データセット
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04673686

反応ノート

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