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Hydrazine hydrate (1:1) → (4-Chloro-3-methoxyphenyl)methanamine

HRID 1934710
ノート
印刷プレビュー

反応式

HRID 1934710 の反応式
[Cl:1][C:2]1[CH:19]=[CH:18][C:5]([CH2:6][N:7]2C(=O)C3=CC=CC=C3C2=O)=[CH:4][C:3]=1[O:20][CH3:21].O.NN>C(O)C>[Cl:1][C:2]1[CH:19]=[CH:18][C:5]([CH2:6][NH2:7])=[CH:4][C:3]=1[O:20][CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 22467651HCID 22467651、化合物

生成物 1

HCID 15548036(4-Chloro-3-methoxyphenyl)methanamine収率 96.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of N-(4-chloro-3-methoxybenzyl)phthalimide (3.00 g) in ethanol (60 mL) was added hydrazine hydrate (2.62 mL), and the mixture was heated for an hour under reflux. The resulting precipitates were faltered off and the filtrate was evaporated in vacuo. The residue was partitioned between chloroform and an aqueous saturated sodium bicarbonate solution. The separated organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo to give 4-chloro-3-methoxybenzylamine as a yellow oil (1.64 g).

後処理

  1. temperaturethe mixture was heated for an hour
  2. temperatureunder reflux
  3. customThe resulting precipitates
  4. customthe filtrate was evaporated in vacuo
  5. customThe residue was partitioned between chloroform
  6. washThe separated organic layer was washed with water and brine
  7. dry with materialdried over magnesium sulfate
  8. customevaporated in vacuo

出典と根拠

ORDレコード
ord-9118fe18302f486b89b864aa13dfd805
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06384080B1

反応ノート

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