Water → HCID 11670326、化合物

HRID 1713027ノート

反応式

HRID 1713027 の反応式
C[O:2][C:3](=[O:34])[CH2:4][N:5]([C:7](=[O:33])[CH2:8][C:9]([CH3:32])([CH3:31])[CH2:10][N:11]1[C:28](=[S:29])[N:14]2[C:15]3[CH:16]=[C:17]([C:21]4[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=4)[O:18][C:19]=3[CH:20]=[C:13]2[C:12]1=[O:30])[CH3:6].O.C(Cl)(Cl)Cl.C([O-])(O)=O.[Na+]>C(O)(C(F)(F)F)=O.CO>[Cl:27][C:24]1[CH:25]=[CH:26][C:21]([C:17]2[O:18][C:19]3[CH:20]=[C:13]4[C:12](=[O:30])[N:11]([CH2:10][C:9]([CH3:31])([CH3:32])[CH2:8][C:7]([N:5]([CH2:4][C:3]([OH:34])=[O:2])[CH3:6])=[O:33])[C:28](=[S:29])[N:14]4[C:15]=3[CH:16]=2)=[CH:22][CH:23]=1

参加物

7

反応物 4

HCID 962Water2 回HCID 6212ChloroformHCID 516892Sodium BicarbonateHCID 11497027HCID 11497027、化合物

生成物 1

HCID 11670326HCID 11670326、化合物収率 88%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
40 °C

実験手順

Compound 20 was dissolved in TFA (1.5 ml) and water (0.75 ml) was added thereto. The resulting mixture was stirred at 40° C. for 16 hours. After cooling the mixture to room temperature, water and chloroform were added, followed by addition of 10% NaHCO3 (20 ml), while maintaining an acidic pH of the solution. The organic layer was separated, washed twice with water, dried over Na2SO4 and the solvent was evaporated under reduced pressure to give an orange solid. Chromatography purification was carried out using with a 8:2 ethyl acetate:methanol mixture as eluent to give Compound 21 (38.3 mg, 88% yield) as a yellow solid.

後処理

  1. temperatureAfter cooling the mixture to room temperature
  2. temperaturewhile maintaining an acidic pH of the solution
  3. customThe organic layer was separated
  4. washwashed twice with water
  5. dry with materialdried over Na2SO4
  6. customthe solvent was evaporated under reduced pressure
  7. customto give an orange solid
  8. customChromatography purification

出典と根拠

ORDレコード
ord-8eae679ba8e841b2903be103be0951a2
出典データセット
uspto-grants-2010_09
特許番号
US07795255B2

反応ノート

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