Hydrochloric Acid → 2-(Aminomethyl)-3,5-di-tert-butylphenol hydrochloride

HRID 1173301ノート

反応式

HRID 1173301 の反応式
Cl.[Cl:2]CC([NH:6][CH2:7][C:8]1[C:13]([OH:14])=[CH:12][C:11]([C:15]([CH3:18])([CH3:17])[CH3:16])=[CH:10][C:9]=1[C:19]([CH3:22])([CH3:21])[CH3:20])=O>C(O)C>[ClH:2].[NH2:6][CH2:7][C:8]1[C:9]([C:19]([CH3:20])([CH3:21])[CH3:22])=[CH:10][C:11]([C:15]([CH3:18])([CH3:17])[CH3:16])=[CH:12][C:13]=1[OH:14]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 687174522-Chloro-N-(2,4-di-tert-butyl-6-hydroxybenzyl)acetamide

生成物 1

HCID 452597712-(Aminomethyl)-3,5-di-tert-butylphenol hydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
85 °C

実験手順

To a solution of 50 mL ethanol and 15 mL conc. hydrochloric acid was added 4.35 g (0.014 mol) of the product of Step A and the reaction mixture was stirred and heated to 85° C. using an external oil bath for 3 h. The reaction mixture was then cooled to room temperature and evaporated in vacuo. Excess water was removed from the product mixture by azeotropic distillation of added portions of toluene on a rotary evaporator. The residue was triturated with ether and dried overnight in vacuo to afford the title compound as a white crystalline solid.

後処理

  1. customfor 3 h
  2. temperatureThe reaction mixture was then cooled to room temperature
  3. customevaporated in vacuo
  4. customExcess water was removed from the product mixture by azeotropic distillation of added portions of toluene on a rotary evaporator
  5. customThe residue was triturated with ether
  6. customdried overnight in vacuo

出典と根拠

ORDレコード
ord-687d2b360f4f4ee79868c9be6a3d7dff
出典データセット
uspto-grants-2010_11
特許番号
US07834062B2

反応ノート

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