HCID 86736409, 화합물 → HCID 12909280, 화합물

HRID 614523노트

반응식

HRID 614523 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:13](C(O)=O)[N:12]2[C:7](=[CH:8][O:9][C:10]3[CH:20]=[CH:19][CH:18]=[CH:17][C:11]=32)[N:6]=1)=[O:4]>C(Cl)(Cl)Cl>[CH:13]1[N:12]2[C:7]([CH2:8][O:9][C:10]3[CH:20]=[CH:19][CH:18]=[CH:17][C:11]=32)=[N:6][C:5]=1[C:3]([O:2][CH3:1])=[O:4]

참가 물질

3

반응물 1

HCID 86736409HCID 86736409, 화합물

생성물 1

HCID 12909280HCID 12909280, 화합물수율 83%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

20 g (0.073 mole) of the 4H-2-methoxycarbonyl-imidazo-[2,1-c][1,4]-benzoxazine-1-carboxylic acid obtained in Step D were added to a flask provided with a magnetic stirrer and the flask was placed in an oil bath at 175°-80° C. Stirring was continued for about twenty minutes until effervescence ceased and the decarboxylated product thus formed was then dissolved in chloroform and the solution obtained was passed down a short silica column to remove any remaining low Rf impurities. The combined fractions containing methyl 4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carboxylate were then evaported to dryness and ether was added with trituration. The offwhite product was filtered off, washed with a little ether and dried to obtain 14.0g (83% yield) of methyl 4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carboxylate with a melting point of 133°-4° C.

후처리

  1. customprovided with a magnetic stirrer
  2. customthe flask was placed in an oil bath at 175°-80° C
  3. waitwas continued for about twenty minutes until effervescence
  4. customthe decarboxylated product thus formed
  5. customthe solution obtained
  6. customto remove any remaining low Rf impurities
  7. additionThe combined fractions containing methyl 4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carboxylate
  8. additionwas added with trituration
  9. filtrationThe offwhite product was filtered off
  10. washwashed with a little ether
  11. customdried

출처 및 근거

ORD 기록
ord-917f2b3f855e402d9b2cdca937c33b9a
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04145419

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