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Sodium Hydroxide → 4-ethylbenzylamine

HRID 1267826
ノート
印刷プレビュー

反応式

HRID 1267826 の反応式
[CH2:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7]([NH2:9])=O)=[CH:5][CH:4]=1)[CH3:2].[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+]>C1COCC1>[CH2:1]([C:3]1[CH:11]=[CH:10][C:6]([CH2:7][NH2:9])=[CH:5][CH:4]=1)[CH3:2]
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

5

反応物 3

HCID 14798Sodium HydroxideHCID 70206224-ethylbenzamideHCID 21226445Aluminium lithium hydride2 回

生成物 1

HCID 38702194-ethylbenzylamine収率 90.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
65 °C

実験手順

A mixture of 4-ethylbenzoic acid (0.50 g, 3.33 mmol) in SOCl2 (1 mL) and DMF(1 drop) was refluxed for 2 h. The reaction mixture was concentrated and then stripped with toluene (2×10 mL) to yield 4-ethylbenzoyl chloride (0.59 g, >100%) as a colorless oil. The crude acid chloride (0.59 g, 3.5 mmol) in toluene (minimum amount) was added dropwise to conc. aq. NH4OH (1.4 mL). After stirring for 1 h, the reaction mixture was concentrated, the residue was dissolved in water and extracted with EtOAc (3×25 mL). The combined organic layers were washed with 1 N aq. NaOH (10 mL) and brine and dried over Na2SO4 prior to removal of the volatiles to yield 4-ethylbenzamide (460 mg, 88%) as a white solid. A suspension of this crude amide (430 mg, 2.87 mmol) and LiAlH4 (180 mg, 4.7 mmol) in dry THF (5 mL) was refluxed at 65° C. for 4.5 h. More LiAlH4 (60 mg, 1.58 mmol) was added, and the reaction mixture was heated at 65° C. for 2 h. The reaction mixture was cooled, and 1 N aq. NaOH (0.4 mL) was added. After stirring for 4 h, the mixture was filtered, and the filtrate was concentrated to give 4-ethylbenzylamine (350 mg, 90w) as a pale yellow oil.

後処理

  1. temperaturethe reaction mixture was heated at 65° C. for 2 h
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe mixture was filtered
  4. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-0cb092a586cd4c25a2c1406a3f87225c
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06555519B2

反応ノート

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