Potassium Carbonate → HCID 19799596、化合物

HRID 974633ノート

反応式

HRID 974633 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[Cl:16])[O:5][CH:6]1[CH2:9][N:8]([C:10](Cl)=[O:11])[CH2:7]1.[CH3:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.C(=O)([O-])[O-].[K+].[K+].[C:30]([OH:37])(=[O:36])/[CH:31]=[CH:32]/[C:33]([OH:35])=[O:34]>O1CCCC1.O.C(O)(C)C>[C:30]([OH:37])(=[O:36])/[CH:31]=[CH:32]/[C:33]([OH:35])=[O:34].[Cl:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[Cl:16])[O:5][CH:6]1[CH2:9][N:8]([C:10]([N:21]2[CH2:22][CH2:23][N:18]([CH3:17])[CH2:19][CH2:20]2)=[O:11])[CH2:7]1

参加物

8

反応物 4

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 444972Fumaric AcidHCID 15042235HCID 15042235、化合物

生成物 1

HCID 19799596HCID 19799596、化合物収率 95.9%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3776Isopropanol溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

A stirred solution of 2.8 g (0.01 mole) of crude 3-(3,4-dichlorophenoxy)-1-azetidinecarbonyl chloride in 25 ml of tetrahydrofuran was treated with 1 g (0.01 mole) of 1-methylpiperazine then with 1.42 g (0.01 mole) of potassium carbonate. After stirring for 30 min, approximately 2 g of ice was added and stirring continued for 18 hr. The reaction mixture was diluted with 200 ml of water and an oil separated. Upon standing, this oil solidified and was collected by filtration, yielding 3.3 g of crude product. The solid was dissolved in 20 ml of isopropanol and treated with 1.16 g of fumaric acid dissolved in 25 ml of boiling isopropanol. The volume was reduced to 30 ml by heating under a stream of nitrogen and upon cooling, the precipitated salt was collected by filtration, yielding 1.35 g (95.9%) of white crystals, m.p. 187°-188° C.

後処理

  1. stirringstirring
  2. waitcontinued for 18 hr
  3. customan oil separated
  4. filtrationwas collected by filtration
  5. customyielding 3.3 g of crude product
  6. temperatureby heating under a stream of nitrogen
  7. temperatureupon cooling
  8. filtrationthe precipitated salt was collected by filtration

出典と根拠

ORDレコード
ord-1cd50ae65b4d4cf994f6fe5a3faffd1d
出典データセット
uspto-grants-1991_11
特許番号
US05068231

反応ノート

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