Acetone → HCID 178476232、化合物
反応式
C[OH:2].Cl.Cl.Cl.[CH2:6]([NH:13][C:14]([NH:16][C:17]([NH:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[NH:18])=[NH:15])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[CH3:30][C:31]([CH3:33])=[O:32]>>[C:31]([OH:2])(=[O:32])[CH3:33].[CH3:30][C:31]1([CH3:33])[N:15]=[C:14]([NH:13][CH2:6][C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:16][C:17]([NH:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[N:18]1参加物
5
実験手順
110 ml of methanol, 80ml of acetone and 0.5 ml of concentrated hydrochloric acid were added to 6.8 g (16.9 mmol) of N1-benzyl-N5-decyl-biguanide dihydrochloride. The mixture was refluxed for 22 hours, and the solvent was distilled off under reduced pressure, and the residue was dissolved in 100 ml of ethanol. To the solution were added 80 ml of water and 7 ml of 5N aqueous sodium hydroxide. The mixture was refluxed for 1.5 hours, concentrated under reduced pressure, and extracted with ethyl acetate. The extract was washed with water, and the solvent was distilled off under reduced pressure. The residue was recrystallized from ethanol/ether to obtain 2.9 g of colorless crystals having a melting point of 106 to 108° C.
後処理
- temperatureThe mixture was refluxed for 22 hours
- distillationthe solvent was distilled off under reduced pressure
- dissolutionthe residue was dissolved in 100 ml of ethanol
- additionTo the solution were added 80 ml of water and 7 ml of 5N aqueous sodium hydroxide
- temperatureThe mixture was refluxed for 1.5 hours
- concentrationconcentrated under reduced pressure
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was recrystallized from ethanol/ether
出典と根拠
- ORDレコード
- ord-b9591d2b59bc47de84bfa0416d40c1aa
- 出典データセット
- uspto-grants-2009_11
- 特許番号
- US07622469B2
反応ノート
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