Hydrochloric Acid → 3-(6-Aminopyridin-3-yl)-2-(1-but-2-ynyl-1H-imidazol-4-yl)propionic acid

HRID 2370942ノート

反応式

HRID 2370942 の反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][CH:9]([C:15]2[N:16]=[CH:17][N:18]([CH2:20][C:21]#[C:22][CH3:23])[CH:19]=2)[C:10]([O:12]CC)=[O:11])=[CH:4][CH:3]=1.[OH-].[Na+].Cl>C1COCC1>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][CH:9]([C:15]2[N:16]=[CH:17][N:18]([CH2:20][C:21]#[C:22][CH3:23])[CH:19]=2)[C:10]([OH:12])=[O:11])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2 回HCID 69331513Ethyl 3-(6-aminopyridin-3-yl)-2-(1-but-2-ynyl-1H-imidazol-4-yl)propionate

生成物 1

HCID 114929383-(6-Aminopyridin-3-yl)-2-(1-but-2-ynyl-1H-imidazol-4-yl)propionic acid収率 22%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 25 mg (0.08 mmol) of the compound from example 32a in 2 ml of THF was mixed with 88 μl of 1N NaOH and stirred at RT for 4 h. Then, and again after stirring overnight, 40 μl of NaOH were added. After stirring for a further 24 h, the reaction mixture was neutralized with 2N HCl and freeze-dried. Preparative HPLC afforded 5 mg of the title compound as bistrifluoroacetate.

後処理

  1. stirringThen, and again after stirring overnight
  2. stirringAfter stirring for a further 24 h
  3. customfreeze-dried

出典と根拠

ORDレコード
ord-cc991dbe73814b228db4d0bf549d0a35
出典データセット
uspto-grants-2014_04
特許番号
US08710232B2

反応ノート

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