Thionyl Chloride → HCID 14067389, 화합물

HRID 614525노트

반응식

HRID 614525 반응식
[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]

참가 물질

3

반응물 2

HCID 24386Thionyl ChlorideHCID 12909281HCID 12909281, 화합물

생성물 1

HCID 14067389HCID 14067389, 화합물수율 83%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-de8aacaa292e44b69b6f78b94c6a08d3
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04145419

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