Boron trifluoride etherate → HCID 178467437, 화합물

HRID 1390308노트

반응식

HRID 1390308 반응식
[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

참가 물질

7

반응물 4

HCID 8000Boron trifluoride etherateHCID 516892Sodium Bicarbonate2회HCID 200293965-Chloropyrimidine-4-carboxylic acidHCID 21329182Ethyl 5-chloropyrimidine-4-carboxylate

생성물 1

HCID 178467437HCID 178467437, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-0ac7c64a8a164223beb0a6a87a27de1a
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04138487

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