HCID 86736409、化合物 → HCID 12909280、化合物

HRID 614523ノート

反応式

HRID 614523 の反応式
[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]

参加物

3

反応物 1

HCID 86736409HCID 86736409、化合物

生成物 1

HCID 12909280HCID 12909280、化合物収率 83%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-917f2b3f855e402d9b2cdca937c33b9a
出典データセット
uspto-grants-1979_03
特許番号
US04145419

反応ノート

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