Hydrochloric Acid → 7-Methoxy-4a-methyl-3,4,4a,9a-tetrahydro[1]benzofuro[2,3-c]pyridine

HRID 1616921

반응식

HRID 1616921 반응식
[CH3:1][O:2][C:3]1[CH:17]=[CH:16][C:6]2[C:7]3([CH3:15])[CH2:12][CH2:11][NH:10][C:9](=O)[CH:8]3[O:14][C:5]=2[CH:4]=1.[AlH4-].[Li+].Cl.[OH-].[Na+]>O1CCCC1.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:17]=[CH:16][C:6]2[C:7]3([CH3:15])[CH2:12][CH2:11][N:10]=[CH:9][CH:8]3[O:14][C:5]=2[CH:4]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 28112Lithium aluminum hydride2회HCID 673237727-methoxy-4a-methyl-3,4,4a,9a-tetrahydro-2Hbenzo[4,5]furo[2,3-c]pyridine-1-one

생성물 1

HCID 673247447-Methoxy-4a-methyl-3,4,4a,9a-tetrahydro[1]benzofuro[2,3-c]pyridine

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매3회HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 7-methoxy-4a-methyl-3,4,4a,9a-tetrahydro-2Hbenzo[4,5]furo[2,3-c]pyridine-1-one (1.0 g, 4.30 mmol) in tetrahydrofuran (3 mL) was slowly added 1.0 M of lithium tetrahydroaluminate in tetrahydrofuran (2 mL). After 30 min stirring another portion of 1.0 M of lithium tetrahydroaluminate in tetrahydrofuran (1 mL) was added and the reaction was stirred for 2 h. The reaction was transferred into ice, 6N aqueous HCl was added followed by ethyl acetate. The aqueous layer was basified by adding NaOH and the product was extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, filtered and the solvent was evaporated to provide a colorless oil. The product was used in the next reaction step without further purification.

후처리

  1. additionwas added
  2. additionwas added
  3. extractionthe product was extracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customthe solvent was evaporated
  8. customto provide a colorless oil
  9. customThe product was used in the next reaction step without further purification

출처 및 근거

ORD 기록
ord-b2c2e0662ec144ac90a842cebd40af0b
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765779B2

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