Hydrochloric Acid → 1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride

HRID 1653702

반응식

HRID 1653702 반응식
[N:1]1[CH:6]=[C:5]([C:7]([OH:9])=[O:8])[CH:4]=[N:3][CH:2]=1.[ClH:10]>O>[ClH:10].[NH:3]1[CH2:4][CH:5]([C:7]([OH:9])=[O:8])[CH2:6][N:1]=[CH:2]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 78346Pyrimidine-5-carboxylic acid

생성물 1

HCID 703421841,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride수율 92.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Pyrimidine-5-carboxylic acid (5.0 g, 40 mmol) was suspended in a mixture of 150 ml water and concentrated hydrochloric acid (4.0 g, 40.5 mmol). The mixture was hydrogenated at 26 psig over 1.0 g Pd-on-carbon 10% in a Parr hydrogenator for 3h. The suspension was filtered and the filter rinsed twice with hot water (20 ml). The filtrate was evaporated in vacuo to give 6.11 g yellow oil (92%). The oil was crystallized from anhydrous methanol/tetrahydrofuran (THF) to give 5.77 g (87%) white crystals in two crops. 300 MHz nmr indicated product.

후처리

  1. filtrationThe suspension was filtered
  2. washthe filter rinsed twice with hot water (20 ml)
  3. customThe filtrate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-087bc02165fc4420a67f9622822fc2f7
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05403845

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