Hydrochloric Acid → 4-[3-(6-Amino-pyridin-3-ylethynyl)-2-methyl-pyridin-4-yl]-benzoic acid

HRID 1529214ノート

反応式

HRID 1529214 の反応式
C[O:2][C:3](=[O:26])[C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][N:13]=[C:12]([CH3:16])[C:11]=2[C:17]#[C:18][C:19]2[CH:20]=[N:21][C:22]([NH2:25])=[CH:23][CH:24]=2)=[CH:6][CH:5]=1.[OH-].[Na+].Cl>C1COCC1>[NH2:25][C:22]1[N:21]=[CH:20][C:19]([C:18]#[C:17][C:11]2[C:12]([CH3:16])=[N:13][CH:14]=[CH:15][C:10]=2[C:7]2[CH:6]=[CH:5][C:4]([C:3]([OH:26])=[O:2])=[CH:9][CH:8]=2)=[CH:24][CH:23]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 582352434-[3-(6-Amino-pyridin-3-ylethynyl)-2-methyl-pyridin-4-yl]-benzoic acid methyl ester

生成物 1

HCID 582353194-[3-(6-Amino-pyridin-3-ylethynyl)-2-methyl-pyridin-4-yl]-benzoic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The title compound is synthesized according to general procedure GP4 starting from 2.0 g (5.8 mmol) 4-[3-(6-amino-pyridin-3-ylethynyl)-2-methyl-pyridin-4-yl]-benzoic acid methyl ester using 11.6 mL (11.6 mmoL) 1 N NaOH in 8 mL THF. After completion of the reaction the pH is adjusted to pH about 5 with 1.0 N HCl. The precipitate is collected by filtration, washed with water and dried under vacuum. The solid is taken up in iPrOH, stirred for a few minutes before the solid is isolated by filtration and dried at 40° C. under vacuum. Yield: 1.9 g (99%).

後処理

  1. customAfter completion of the reaction the pH
  2. filtrationThe precipitate is collected by filtration
  3. washwashed with water
  4. customdried under vacuum
  5. customis isolated by filtration
  6. customdried at 40° C. under vacuum

出典と根拠

ORDレコード
ord-dabc0a9d1e104228a4fbca9ef413c19f
出典データセット
uspto-grants-2015_07
特許番号
US09090564B2

反応ノート

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