Sodium Hydroxide → HCID 131732142、化合物

HRID 1400078ノート

反応式

HRID 1400078 の反応式
NO.Cl.[OH-].[Na+].CC1[N:8]([C@H:13]2[CH2:20][C@@:19]3([C:21]([O:23][CH2:24][C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)=[O:22])[C@H:15]([CH2:16][CH2:17][CH2:18]3)[CH2:14]2)C(C)=CC=1>O.CO>[NH2:8][C@H:13]1[CH2:20][C@@:19]2([C:21]([O:23][CH2:24][C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)=[O:22])[C@H:15]([CH2:16][CH2:17][CH2:18]2)[CH2:14]1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 131732143HCID 131732143、化合物

生成物 1

HCID 131732142HCID 131732142、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

反応条件

温度
65 °C

実験手順

To a aqueous solution of NH2OH.HCl (8.4 g, 121.2 mmol) and NaOH (2.2 g, 19.54 mmol) in H2O (20 mL) was added a solution of Example 48C (2.81 g, 8.36 mmol) in MeOH (70 mL) and the mixture was heated at 65° C. for 8 hours. The mixture was cooled to room temperature, sufficient water was added and MeOH was removed under reduced pressure. The resulting slurry was adjusted to pH=10 with NaOH solution (2.5 N) and extracted with dichloromethane. The combined organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated to give a crude product, which was purified by column chromatography (SiO2, dichloromethane:MeOH from 100:1 to 10:1) to get the title compound.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. customMeOH was removed under reduced pressure
  3. extractionextracted with dichloromethane
  4. washThe combined organic layer was washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give a crude product, which
  9. customwas purified by column chromatography (SiO2, dichloromethane:MeOH from 100:1 to 10:1)

出典と根拠

ORDレコード
ord-08a65a1261474907988c5d5c461e5fb4
出典データセット
uspto-grants-2014_12
特許番号
US08906911B2

反応ノート

読み込み中…