1-Methyl-3-triphenylmethyl-5-methoxycarbonyl-1,4,5,6-tetrahydropyrimidinium iodide → 1-Methyl-5-methoxycarbonyl-1,4,5,6-tetrahydropyrimidine

HRID 1681899노트

반응식

HRID 1681899 반응식
[I-].[CH3:2][NH+:3]1[CH2:8][CH:7]([C:9]([O:11][CH3:12])=[O:10])[CH2:6][N:5](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH2:4]1>C(O)(C(F)(F)F)=O>[CH3:2][N:3]1[CH2:8][CH:7]([C:9]([O:11][CH3:12])=[O:10])[CH2:6][N:5]=[CH:4]1

참가 물질

3

반응물 1

HCID 867464331-Methyl-3-triphenylmethyl-5-methoxycarbonyl-1,4,5,6-tetrahydropyrimidinium iodide

생성물 1

HCID 152943851-Methyl-5-methoxycarbonyl-1,4,5,6-tetrahydropyrimidine

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매2회

실험 절차

1-Methyl-3-triphenylmethyl-5-methoxycarbonyl-1,4,5,6-tetrahydropyrimidinium iodide (395 mg, 0.75 mmol) is dissolved in TFA (1 ml) with stirring in a stoppered round bottom flask at room temperature. After 18 hours stirring the excess TFA is evaporated in vacuo, and the dark residue triturated with ether. The ether is decanted leaving an oily residue that is taken up in ice cold sat. Na2CO3 and then extracted with chloroform. After drying and evaporation the chloroform fraction gave the free base which is recrystallized (chloroform/hexane) to yellow crystals 88 mg (74%) identified by 300 MHz nmr, ms m/z=156.

후처리

  1. customis evaporated in vacuo
  2. customthe dark residue triturated with ether
  3. customThe ether is decanted
  4. customleaving an oily residue that
  5. extractionextracted with chloroform
  6. customAfter drying
  7. customevaporation the chloroform fraction
  8. customgave the free base which
  9. customis recrystallized (chloroform/hexane) to yellow crystals 88 mg (74%)

출처 및 근거

ORD 기록
ord-1b1b3693cd5f46c689e3e567c4b61b19
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05175166

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