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Triethylamine → 1-(2,6-Dichloro-5-fluoro-4-pyrimidinyl)-3-methyl-3-pyrrolidinol

HRID 1366521
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HRID 1366521 반응식
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([F:9])=[C:4](Cl)[N:3]=1.C(N(CC)CC)C.[CH3:18][C:19]1([OH:24])[CH2:23][CH2:22][NH:21][CH2:20]1>C1COCC1.CO>[Cl:1][C:2]1[N:3]=[C:4]([N:21]2[CH2:22][CH2:23][C:19]([CH3:18])([OH:24])[CH2:20]2)[C:5]([F:9])=[C:6]([Cl:8])[N:7]=1
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 133889932,4,6-Trichloro-5-fluoropyrimidineHCID 145784583-Methylpyrrolidin-3-ol

생성물 1

HCID 866369741-(2,6-Dichloro-5-fluoro-4-pyrimidinyl)-3-methyl-3-pyrrolidinol수율 77.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

To a solution of 2,4,6-trichloro-5-fluoropyrimidine (0.476 g, 2.36 mmol) and triethylamine (0.36 mL, 2.60 mmol) in THF was added 3-methyl-3-pyrrolidinol (0.239 g, 2.36 mmol) in THF and MeOH (2 mL). The reaction was stirred at room temperature for 2.5 hours, and then the solvent was removed in vacuo. Water was added to the residue, and the mixture was extracted with ethyl acetate. The organics were dried (Na2SO4) and evaporated to provide 1-(2,6-dichloro-5-fluoro-4-pyrimidinyl)-3-methyl-3-pyrrolidinol as an orange solid (0.486 g, 77%). LCMS: (M+H)+=266.1.

후처리

  1. customthe solvent was removed in vacuo
  2. additionWater was added to the residue
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe organics were dried (Na2SO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-7351a1117ce24f539e5a4271bdaea714
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07893056B2

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