Hydrogen Bromide → HCID 20080417、化合物

HRID 1681868

反応式

HRID 1681868 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[N:7][CH:8]=[N:9][CH:10]=1)=[O:4].[BrH:11]>>[BrH:11].[CH3:1][O:2][C:3]([CH:5]1[CH2:10][NH:9][CH:8]=[N:7][CH2:6]1)=[O:4]

参加物

3

反応物 2

HCID 260Hydrogen BromideHCID 253902Methyl pyrimidine-5-carboxylate

生成物 1

HCID 20080417HCID 20080417、化合物収率 83%

実験手順

5-Methoxycarbonylpyrimidine (1.381 g, 10 mmol) in 143 ml 0.07158M HBr was hydrogenated at 26 psig over 600 mg Pd-on-carbon 10% in a Parr hydrogenator for three hours. The suspension was filtered and the filter rinsed twice with hot water (10 ml). The filtrate was evaporated in vacuo to give 1.86 g yellow oil (83%). The oil was crystallized from anhydrous ethanol/THF, and the hygroscopic crystals collected by decanting the solvents under a stream of nitrogen. Excess solvents were removed under vacuum in a drying pistol to yield 1.01 g (45%) white crystals mp 149°-153° C. (with the evolution of gas). Microanalysis calc.: C 32.3, H 4.97, N 12.56; found: C 32.12, H 5.15, N 12.34. 400 MHz nmr indicated product.

後処理

  1. filtrationThe suspension was filtered
  2. washthe filter rinsed twice with hot water (10 ml)
  3. customThe filtrate was evaporated in vacuo

出典と根拠

ORDレコード
ord-252490bec2b94d89a744d9bfb7891266
出典データセット
uspto-grants-1992_12
特許番号
US05175166

関連ノート

読み込み中…