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Methyl p-toluenesulfonate → HCID 86616753, 화합물

HRID 2243776
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HRID 2243776 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]([CH2:9][CH2:10][OH:11])[C:4](=[O:12])[N:3]=1.[C:13]1([CH3:24])[CH:18]=[CH:17][C:16]([S:19]([O:22]C)(=[O:21])=[O:20])=[CH:15][CH:14]=1>C(#N)C>[C:13]1([CH3:24])[CH:14]=[CH:15][C:16]([S:19]([O-:22])(=[O:20])=[O:21])=[CH:17][CH:18]=1.[OH:11][CH2:10][CH2:9][NH+:5]1[C:6]([CH3:8])=[CH:7][CH:2]([CH3:1])[N:3]([CH3:13])[C:4]1=[O:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6645Methyl p-toluenesulfonateHCID 1219311-(2-Hydroxyethyl)-4,6-dimethyl-2(1H)-pyrimidinone

생성물 1

HCID 86616753HCID 86616753, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
0 °C

실험 절차

Under a protective-gas atmosphere, a mixture of 9.2 g (0.055 mol) of 4,6-dimethyl-1-(2-hydroxyethyl)pyrimidin-2(1H)-one and 13.1 g (0.068 mol) of methyl p-toluenesulfonate in 700 ml of acetonitrile was heated under reflux for 12 hours. After cooling, about ⅔ of the solvent was removed on a rotary evaporator, the remaining residue was mixed with the same amount of diethyl ether and cooled to 0° C. At low temperature, firstly an oil separated off, which crystallized out after some time. The crystalline product was filtered off.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 12 hours
  3. temperatureAfter cooling, about ⅔ of the solvent
  4. customwas removed on a rotary evaporator
  5. additionthe remaining residue was mixed with the same amount of diethyl ether
  6. customAt low temperature, firstly an oil separated off
  7. customwhich crystallized out after some time
  8. filtrationThe crystalline product was filtered off

출처 및 근거

ORD 기록
ord-fdcbdba07d8c45e29f3e7e93261f45b5
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07678156B2

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