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

HRID 1366521
ノート
印刷プレビュー

反応式

HRID 1366521 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7351a1117ce24f539e5a4271bdaea714
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07893056B2

反応ノート

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