Sodium Hydroxide → HCID 131732142, 화합물

HRID 1400078노트

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HRID 1400078 반응식
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

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 131732143HCID 131732143, 화합물

생성물 1

HCID 131732142HCID 131732142, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

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온도
65 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-08a65a1261474907988c5d5c461e5fb4
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08906911B2

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