Boron trifluoride etherate → HCID 178467437、化合物

HRID 1390308ノート

反応式

HRID 1390308 の反応式
[Cl:1][C:2]1[C:3](C(OCC)=O)=[N:4][CH:5]=[N:6][CH:7]=1.ClC1[C:15]([C:20]([OH:22])=O)=NC=NC=1.B(F)(F)F.C[CH2:28][O:29]CC.C(=O)(O)[O-].[Na+]>C(Cl)Cl.C(O)C>[Cl:1][C:2]1[C:3]([O:22][CH2:20][CH3:15])=[N:4][C:5](=[C:28]=[O:29])[NH:6][CH:7]=1

参加物

7

反応物 4

HCID 8000Boron trifluoride etherateHCID 516892Sodium Bicarbonate2 回HCID 200293965-Chloropyrimidine-4-carboxylic acidHCID 21329182Ethyl 5-chloropyrimidine-4-carboxylate

生成物 1

HCID 178467437HCID 178467437、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒

実験手順

5-Chloro-4-ethoxycarbonylpyrimidine can be prepared by treating 5-chloro-4-carboxypyrimidine (40 g) with ethanol (400 cc) and boron trifluoride etherate (80 cc). After heating for 24 hours under reflux, the volatile materials are eliminated and then methylene chloride (250 cc) is added. An 8% (w/v) aqueous sodium bicarbonate solution (100 cc) is added and then the pH is adjusted to 6 by the addition of sodium bicarbonate powder. A further extraction is carried out with methylene chloride (300 cc). The solvent is evaporated off and then the residue distilled. 5-Chloro-4-ethoxy-carbonylpyrimidine (23 g), b.p. 132°-133° C./33 mm Hg, is obtained.

後処理

  1. temperatureAfter heating for 24 hours
  2. temperatureunder reflux
  3. extractionA further extraction
  4. customThe solvent is evaporated off
  5. distillationthe residue distilled

出典と根拠

ORDレコード
ord-0ac7c64a8a164223beb0a6a87a27de1a
出典データセット
uspto-grants-1979_02
特許番号
US04138487

反応ノート

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