Monomethylamine methanol → 4-aminomethyl-N-(4-dipropylaminobutyl)benzenesulfonamide

HRID 348609ノート

反応式

HRID 348609 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[CH2:12][C:13]1[CH:18]=[CH:17][C:16]([S:19]([NH:22][CH2:23][CH2:24][CH2:25][CH2:26][N:27]([CH2:31][CH2:32][CH3:33])[CH2:28][CH2:29][CH3:30])(=[O:21])=[O:20])=[CH:15][CH:14]=1.CN.CO>>[NH2:3][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([S:19]([NH:22][CH2:23][CH2:24][CH2:25][CH2:26][N:27]([CH2:31][CH2:32][CH3:33])[CH2:28][CH2:29][CH3:30])(=[O:20])=[O:21])=[CH:15][CH:14]=1

参加物

3

反応物 2

HCID 57454252Monomethylamine methanolHCID 669411664-(1,3-dioxo-1,3-dihydroisoindol-2-ylmethyl)-N-(4-dipropylaminobutyl)benzenesulfonamide

生成物 1

HCID 230792764-aminomethyl-N-(4-dipropylaminobutyl)benzenesulfonamide収率 98.4%

実験手順

The compound (160 mg) obtained in Example 24-3 was added with 2.0 ml of a 40% methylamine/methanol solution (manufactured by Tokyo Kasei Kogyo Co., Ltd.), followed by stirring at room temperature for 40 hours. After completion of the reaction, the solvent was distilled off and the residue was subjected to extraction by the addition of a 1 mol/l sodium hydroxide aqueous solution and chloroform. The organic layer was dried with anhydrous sodium sulfate and the solvent was distilled off, thereby obtaining the subject compound (114 mg) as a colorless viscous liquid.

後処理

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off
  3. extractionthe residue was subjected to extraction by the addition of a 1 mol/l sodium hydroxide aqueous solution and chloroform
  4. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  5. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-1d4b603b8d984a1faf4bfa0c9fffb753
出典データセット
uspto-grants-2007_02
特許番号
US07176227B2

反応ノート

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