Sodium Hydroxide → 3-(2-Dimethylamino-ethoxy)-4-methylaniline

HRID 914963

反応式

HRID 914963 の反応式
[CH3:1][N:2]([CH3:21])[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([NH:13]C(=O)OC(C)(C)C)[CH:9]=[CH:10][C:11]=1[CH3:12].[OH-].[Na+]>Cl>[CH3:1][N:2]([CH3:21])[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH:9]=[CH:10][C:11]=1[CH3:12])[NH2:13]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 71166994tert-Butyl (3-(2-dimethylamino-ethoxy)-4-methyl-phenyl)-carbamate

生成物 1

HCID 392392273-(2-Dimethylamino-ethoxy)-4-methylaniline収率 89.6%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of 8 (1.15 g) in 6N HCl (10 mL) was heated at 60° C. for 4 hours. After cooling to room temperature, the solution was neutralized with 6N NaOH solution. The aqueous mixture was extracted with EtOAc (2×30 mL), the combined organic layers were washed with brine (1×50 mL) and dried over MgSO4. The solids were filtered, and the filtrate was concentrated under reduced pressure to give the desired product as an oil (0.68 g).

後処理

  1. extractionThe aqueous mixture was extracted with EtOAc (2×30 mL)
  2. washthe combined organic layers were washed with brine (1×50 mL)
  3. dry with materialdried over MgSO4
  4. filtrationThe solids were filtered
  5. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-33783928e7394abaad2990d869dbd759
出典データセット
uspto-grants-2007_09
特許番号
US07265122B2

関連ノート

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