Methanol → 2-Methoxy-6-methylpyrimidine-4-carboxylic acid

HRID 2069383ノート

反応式

HRID 2069383 の反応式
C[O:2][C:3]([C:5]1[CH:10]=[C:9]([CH3:11])[N:8]=[C:7](Cl)[N:6]=1)=[O:4].[CH3:13][OH:14]>[OH-].[Na+]>[CH3:13][O:14][C:7]1[N:6]=[C:5]([C:3]([OH:2])=[O:4])[CH:10]=[C:9]([CH3:11])[N:8]=1

参加物

4

反応物 2

HCID 887MethanolHCID 2736835Methyl 2-chloro-6-methylpyrimidine-4-carboxylate

生成物 1

HCID 190184722-Methoxy-6-methylpyrimidine-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A suspension of methyl-2-chloro-6-methylpyrimidine-4-carboxylate (5.0 g) in 2N aq. NaOH (67 mL) and methanol (67 mL) is stirred at rt for 24 h. Methanol is evaporated and the aq. phase is acidified with 25% aq. HCl at 0° C. A beige crystalline solid crushes out. It is filtered, rinsed with water and heptane and dried (3.0 g); LC-MS: tR=0.55 min, [M+H]+=169.01; 1H NMR (D6-DMSO): δ 2.50 (s, 3H), 3.94 (s, 3H), 7.52 (s, 1H), 13.7 (s br, 1H).

後処理

  1. customMethanol is evaporated
  2. customis acidified with 25% aq. HCl at 0° C
  3. filtrationIt is filtered
  4. washrinsed with water and heptane
  5. customdried (3.0 g)

出典と根拠

ORDレコード
ord-b46050ff1e964b5ea06008e685357766
出典データセット
uspto-grants-2012_10
特許番号
US08299086B2

反応ノート

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