Methyl Methanesulfonate → 1-(2-Hydroxyethyl)-2-methylthio-3,4,5,6-tetrahydropyrimidine mesylate

HRID 256538

반응식

HRID 256538 반응식
[OH:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][CH2:7][NH:6][C:5]1=[S:10].[CH3:11][S:12]([O:15]C)(=[O:14])=[O:13]>C(O)C.COC(C)(C)C>[S:12]([OH:15])(=[O:14])(=[O:13])[CH3:11].[OH:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][CH2:7][NH:6][CH:5]1[S:10][CH3:11]

참가 물질

5

반응물 2

HCID 4156Methyl MethanesulfonateHCID 36032811-(2-Hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione

생성물 1

HCID 867473441-(2-Hydroxyethyl)-2-methylthio-3,4,5,6-tetrahydropyrimidine mesylate수율 128.8%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 15413tert-Butyl methyl ether용매

실험 절차

Then, 1-(2-hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione (121.2 g) and methyl methanesulfonate (91.51 g) are heated at reflux in ethyl alcohol (200 ml) for about 2 hours and then allowed to cool to room temperature. The mixture was diluted with t-butyl methyl ether (2 liters). An oil separates which crystallizes on keeping in freezer at -20° C. Filtration and drying yields 145.7 g of 1-(2-hydroxyethyl)-2-methylthio-3,4,5,6-tetrahydropyrimidine mesylate, melting point 61.7°-62.2° C.

후처리

  1. customAn oil separates which crystallizes
  2. customon keeping in freezer at -20° C
  3. filtrationFiltration
  4. customdrying

출처 및 근거

ORD 기록
ord-333625bfe3524323baec2a941c41e1f7
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258381

연결된 노트

불러오는 중…