Triethylamine → N-([(7S)-3, 4-Dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]-methyl}-2,2,2-trifluoroacetamide

HRID 657542노트

반응식

HRID 657542 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C@@H:7]([CH2:13][NH2:14])[CH2:6]2.C(N(CC)CC)C.[F:22][C:23]([F:30])([F:29])[C:24](OCC)=[O:25]>CO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C@@H:7]([CH2:13][NH:14][C:24](=[O:25])[C:23]([F:30])([F:29])[F:22])[CH2:6]2

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 9794Ethyl trifluoroacetateHCID 115066164,5-Dimethoxy-1-(aminomethyl)benzocyclobutane, (S)-

생성물 1

HCID 86628625N-([(7S)-3, 4-Dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]-methyl}-2,2,2-trifluoroacetamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To 2.9 g (15 mmol) of {[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]methyl}amine in 7.5 mL of methanol, at ambient temperature, there are added, all at once, 2.1 mL (15 mmol/1 eq.) of triethylamine, and then, dropwise, over 20 minutes, 2.3 mL (19 mmol/1.25 eq.) of ethyl trifluoroacetate. Stirring is carried out at ambient temperature for 2 hours, followed by evaporating to dryness. The residue is taken up in 100 mL of dichloromethane, and washing with 50 mL of 1N hydrochloric acid and then 50 mL of water and drying over magnesium sulphate are carried out. After filtration and concentration, the desired product is collected.

후처리

  1. customby evaporating to dryness
  2. washwashing with 50 mL of 1N hydrochloric acid
  3. dry with material50 mL of water and drying over magnesium sulphate
  4. filtrationAfter filtration and concentration
  5. customthe desired product is collected

출처 및 근거

ORD 기록
ord-1f9e5c1d61c145b38d29b5dd563bf9c6
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076325B2

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