반응 #1740888

반응 방정식

benzyl alcohol

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride

thionyl chloride

ethyl ether

→

product

수율 76.0%

Benzyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride

수율 76.0%

반응 조건

후처리

1. 1
   기타precipitation
2. 2
   기타The white solids were collected
3. 3
   기타crystallized from methanol/THF

실험 절차

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.0 g, 6.1 mmol) was suspended in dry benzyl alcohol (20 ml). To the mixture was added thionyl chloride (0.76 g, 6.39 mmol) and the resulting mixture was heated in an oil bath at 80° C. for 24h. The clear solution was poured to anhydrous ethyl ether (100 ml) to induce precipitation. The white solids were collected and crystallized from methanol/THF to give 1.18 g (76%) of product (mp 113°-114° C.). 300 MHz nmr indicated the product. Microanalysis calc.: C 56.58, H 5.89, N 11.00; found: C 56.34, H 6.03, N 11.19.

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