2-Butanamine, 2-methyl- → 1-(3,4-Dichlorophenyl)-2-(tert-amylamino)ethanol hydrochloride

HRID 482288ノート

反応式

HRID 482288 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]([OH:12])[CH2:10]Br)[CH:5]=[CH:6][C:7]=1[Cl:8].[CH3:13][C:14]([NH2:18])([CH2:16][CH3:17])[CH3:15]>C(O)C>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]([OH:12])[CH2:10][NH:18][C:14]([CH2:16][CH3:17])([CH3:15])[CH3:13])[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

4

反応物 2

HCID 689862-Butanamine, 2-methyl-HCID 3441362-Bromo-1-(3,4-dichlorophenyl)ethanol

生成物 1

HCID 190639411-(3,4-Dichlorophenyl)-2-(tert-amylamino)ethanol hydrochloride収率 78%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

27 g (0.1 mol) of 1-(3,4-dichlorophenyl)-2-bromoethanol are added in the cold state to a solution of 37.5 g (50 ml) (0.43 mol) of 2-methyl-2-butylamine, 100 ml of ethanol and 0.5 g of KI. After 48 hours in contact at 20° C. and 3 hours under reflux, the mixture is filtered, the filtrate is evaporated under vacuum, the residue is taken up with ether and the organic phase is washed with water. 200 ml of N HCl are added, and the product is drained and washed with 20 ml of cold water and with ether. The hydrochloride (m.p.=184°-185° C.) is obtained in a 78% yield.

後処理

  1. temperature3 hours under reflux
  2. filtrationthe mixture is filtered
  3. customthe filtrate is evaporated under vacuum
  4. washthe organic phase is washed with water
  5. addition200 ml of N HCl are added
  6. washwashed with 20 ml of cold water and with ether

出典と根拠

ORDレコード
ord-1241d34b6f0e4d53bdaf40758f3b2004
出典データセット
uspto-grants-1998_08
特許番号
US05795915

反応ノート

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