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7-benzenesulfonyl-3,4-dihydro-2H-naphthalen-1-one → C-(6-Benzenesulfonyl-naphthalen-1-yl)-methylamine

HRID 1715060
ノート
印刷プレビュー

反応式

HRID 1715060 の反応式
[C:1]1([S:7]([C:10]2[CH:19]=[C:18]3[C:13]([CH2:14][CH2:15][CH2:16][C:17]3=O)=[CH:12][CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:21]1([S:27]([C:30]2[CH:31]=[C:32]3[C:37](=[CH:38][CH:39]=2)[C:36]([CH2:40][NH2:41])=[CH:35][CH:34]=[CH:33]3)(=[O:29])=[O:28])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.Cl.[CH3:43][C:44]1([CH3:52])[CH2:49][NH:48][CH:47](SC)[NH:46][CH2:45]1>C(Cl)Cl>[C:21]1([S:27]([C:30]2[CH:31]=[C:32]3[C:37](=[CH:38][CH:39]=2)[C:36]([CH2:40][NH2:41])=[CH:35][CH:34]=[CH:33]3)(=[O:29])=[O:28])[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1.[C:1]1([S:7]([C:10]2[CH:19]=[C:18]3[C:13]([CH:14]=[CH:15][CH:16]=[C:17]3[CH2:40][NH:41][C:47]3[NH:46][CH2:45][C:44]([CH3:52])([CH3:43])[CH2:49][N:48]=3)=[CH:12][CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 590217777-benzenesulfonyl-3,4-dihydro-2H-naphthalen-1-oneHCID 59028770C-(6-Benzenesulfonyl-naphthalen-1-yl)-methylamineHCID 666515215,5-Dimethyl-2-methylsulfanyl-hexahydro-pyrimidine hydrochloride

生成物 2

HCID 59028770C-(6-Benzenesulfonyl-naphthalen-1-yl)-methylamineHCID 59028791(7-Benzenesulfonyl-naphthalen-1-ylmethyl)-(5,5-dimethyl-1,4,5,6-tetrahydro-pyrimidin-2-yl)-amine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
150 °C

実験手順

C-(6-Benzenesulfonyl-naphthalen-1-yl)-methylamine is prepared from 7-Benzenesulfonyl-3,4-dihydro-2H-naphthalen-1-one following the procedures of Examples 1 and 2. C-(6-Benzenesulfonyl-naphthalen-1-yl)-methylamine and 5,5-dimethyl-2-methylsulfanyl-hexahydro-pyrimidine hydrochloride are added to methylene chloride, and the reaction mixture is heated to gentle reflux until all of the solvent is evaporated. The reaction mixture is heated to 150° C. and then cooled. The resulting mixture is basified by dropwise addition of aqueous NaOH solution, and then purified by preparative liquid chromatography to give (7-benzenesulfonyl-naphthalen-1-ylmethyl)-(5,5-dimethyl-1,4,5,6-tetrahydro-pyrimidin-2-yl)-amine.

後処理

  1. temperaturethe reaction mixture is heated
  2. temperatureto gentle reflux until all of the solvent
  3. customis evaporated
  4. temperaturecooled
  5. additionThe resulting mixture is basified by dropwise addition of aqueous NaOH solution
  6. custompurified by preparative liquid chromatography

出典と根拠

ORDレコード
ord-bbf763555e034b0d90faa2dd2f9e014a
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07799797B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート