Hydroxyamine hydrochloride → HCID 136388571, 화합물

HRID 966404노트

반응식

HRID 966404 반응식
[C:1]([C:4]1[C:14]([OH:15])=[CH:13][C:12]2[CH:11]3[CH2:16][CH:7]([CH2:8][N:9]([C:17](=[O:22])[C:18]([F:21])([F:20])[F:19])[CH2:10]3)[C:6]=2[CH:5]=1)(=O)[CH3:2].Cl.[NH2:24][OH:25].CC([O-])=O.[Na+]>CO.O>[F:20][C:18]([F:21])([F:19])[C:17]([N:9]1[CH2:10][CH:11]2[CH2:16][CH:7]([C:6]3[CH:5]=[C:4]([C:1](=[N:24][OH:25])[CH3:2])[C:14]([OH:15])=[CH:13][C:12]=32)[CH2:8]1)=[O:22]

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 218647091-(4-Acetyl-5-hydroxy-10-aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-2,2,2-trifluoro-ethanone

생성물 1

HCID 136388571HCID 136388571, 화합물수율 93%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

1-(4-Acetyl-5-hydroxy-10-aza-tricyclo[6.3.1.02.7]dodeca-2(7),3,5-trien-10-yl)-2,2,2-trifluoro-ethanone (190 mg, 0.605 mmol), hydroxylamine HCl (99 mg, 1.21 mmol) and NaOAc (118 mg, 1.21 mmol) were combined in MeOH (4 mL) and H2O (1 mL) and warmed to 65° C. for 18 hours. The mixture was cooled, diluted with H2O and extracted with EtOAc which was dried (Na2SO4), filtered and concentrated to provide a yellow oil (177 mg, 93%).

후처리

  1. temperatureThe mixture was cooled
  2. extractionextracted with EtOAc which
  3. dry with materialwas dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d07645b6acc64ee589e9b2f45fc3762e
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06951938B2

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