Sodium Carbonate → 8-Amino-1-tetralone

HRID 9261

반응식

HRID 9261 반응식
[O:1]=[C:2]1[C:11]2[C:10]([NH:12]C(=O)C)=[CH:9][CH:8]=[CH:7][C:6]=2[CH2:5][CH2:4][CH2:3]1.C([O-])([O-])=O.[Na+].[Na+].[OH-].[Na+]>Cl>[NH2:12][C:10]1[CH:9]=[CH:8][CH:7]=[C:6]2[C:11]=1[C:2](=[O:1])[CH2:3][CH2:4][CH2:5]2

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 12119265N-(8-Oxo-5,6,7,8-tetrahydronaphthalen-1-YL)acetamide

생성물 1

HCID 114009428-Amino-1-tetralone수율 56%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

The amide (Intermediate J2, 4.12 g, 20.3 mmol) was heated at 90° C. in 6N HCl (140 mL) for 3 h. The mixture was cooled to rt and Na2CO3 was added in small portions followed by addition of 2N NaOH until the mixture was at pH 8. The aqueous layer was extracted with EtOAc and the organic fractions were combined, washed with brine, dried, filtered and concentrated to give 8-amino-3,4-dihydro-2H-naphthalen-1-one (Intermediate J3) as a dark red solid 1.82 g (56%).

후처리

  1. extractionThe aqueous layer was extracted with EtOAc
  2. washwashed with brine
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-cb8706557d35427e999736d01fcd803a
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091232B2

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