Thionyl Chloride → HCID 14067389、化合物

HRID 614525ノート

反応式

HRID 614525 の反応式
[CH:1]1[N:9]2[C:4]([CH2:5][O:6][C:7]3[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=32)=[N:3][C:2]=1[C:14]([OH:16])=O.S(Cl)([Cl:19])=O>>[CH:1]1[N:9]2[C:4]([CH2:5][O:6][C:7]3[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=32)=[N:3][C:2]=1[C:14]([Cl:19])=[O:16]

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 12909281HCID 12909281、化合物

生成物 1

HCID 14067389HCID 14067389、化合物収率 83%

実験手順

5 g (0.023 mole) of 4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carboxylic acid were suspended in 15 ml of thionyl chloride and the mixture obtained was refluxed for two hours during which time the solid material completely dissolved. Excess thionyl chloride was removed by azeotroping with benzene on a rotary evaporator and the product was triturated with ether, filtered off and dried to obtain 4.5 g (83% yield of 4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carbonyl chloride with a melting point of 240° C. (decomp).

後処理

  1. customthe mixture obtained
  2. temperaturewas refluxed for two hours during which time the solid material
  3. dissolutioncompletely dissolved
  4. customExcess thionyl chloride was removed
  5. customby azeotroping with benzene on a rotary evaporator
  6. customthe product was triturated with ether
  7. filtrationfiltered off
  8. customdried

出典と根拠

ORDレコード
ord-de8aacaa292e44b69b6f78b94c6a08d3
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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