Water → HCID 178519778、化合物

HRID 1943688ノート

反応式

HRID 1943688 の反応式
C([O:8][C:9]1[CH:13]=[C:12]([C:14]([N:16]2[CH2:21][CH2:20][O:19][C:18]3[CH:22]=[CH:23][N:24]=[CH:25][C:17]2=3)=[O:15])[O:11][N:10]=1)C1C=CC=CC=1.O.C(=O)([O-])O.[Na+]>Br.C(O)(=O)C>[O:19]1[CH2:20][CH2:21][N:16]([C:14]([C:12]2[O:11][N:10]=[C:9]([OH:8])[CH:13]=2)=[O:15])[C:17]2[CH:25]=[N:24][CH:23]=[CH:22][C:18]1=2

参加物

6

反応物 3

HCID 962WaterHCID 516892Sodium BicarbonateHCID 66936639HCID 66936639、化合物

生成物 1

HCID 178519778HCID 178519778、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 260Hydrogen Bromide溶媒

実験手順

In 3 ml of 33% hydrobromic acid in acetic acid solution, (3-benzyloxy -isoxazol-5-yl)-(2,3-dihydro-pyrido[4,3-b][1,4]oxazin-4-yl)-methanone (45 mg, 0.13 mmol) was dissolved and then stirred at room temperature for 24 hours. After completion of the reaction by adding water dropwise, the mixture was adjusted to weak acidic condition (pH=6) by using saturated solution of sodium hydrogen carbonate and extracted with ethyl acetate. The aqueous layer was evaporated under reduced pressure and the residue was purified by using preparative TLC plate to obtain the target compound 44, i.e., (2,3-dihydro-pyrido[4,3-b][1,4]oxazin-4-yl)-(3-hydroxy-isoxazol-5-yl)-methanone, as white solid (8 mg, 24%).

後処理

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. customThe aqueous layer was evaporated under reduced pressure
  4. customthe residue was purified

出典と根拠

ORDレコード
ord-2de8ee52154f48b4a8ad3de5a6866b2c
出典データセット
uspto-grants-2013_03
特許番号
US08394792B2

反応ノート

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