Hydrogen Bromide → HCID 20080417, 화합물

HRID 1681868

반응식

HRID 1681868 반응식
[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]

참가 물질

3

반응물 2

HCID 260Hydrogen BromideHCID 253902Methyl pyrimidine-5-carboxylate

생성물 1

HCID 20080417HCID 20080417, 화합물수율 83%

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-252490bec2b94d89a744d9bfb7891266
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05175166

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