Sodium Hydroxide → 2-(1-Trityl-1H-imidazol-4-yl)-ethylamine

HRID 412168ノート

反応式

HRID 412168 の反応式
[C:1]1([C:7]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:8]2[CH:12]=[C:11]([CH2:13][CH2:14][NH:15]C(=O)C(F)(F)F)[N:10]=[CH:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+]>CO>[C:28]1([C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[N:8]2[CH:12]=[C:11]([CH2:13][CH2:14][NH2:15])[N:10]=[CH:9]2)[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

参加物

4

反応物 2

HCID 14798Sodium Hydroxide2 回HCID 110377171-(Triphenylmethyl)-4-[2-(trifluoroacetamido)-1-ethyl]imidazole

生成物 1

HCID 6183402-(1-Trityl-1H-imidazol-4-yl)-ethylamine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of the product from Step A (48.8 g, 109 mmol) in 1L of methanol was added 1M sodium hydroxide solution (325 mL, 325 mmol). Over the course of four days, additional methanol (3 L) and sodium hydroxide solution (325 mL, 325 mmol) were added. The solution was concentrated in vacuo, and partitioned between EtOAc and water. The organic layer was washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo to provide the titled product.

後処理

  1. concentrationThe solution was concentrated in vacuo
  2. custompartitioned between EtOAc and water
  3. washThe organic layer was washed with brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c59ea682f89c4f60ab0002448724a62f
出典データセット
uspto-grants-2003_05
特許番号
US06562823B1

反応ノート

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