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

HRID 657542ノート

反応式

HRID 657542 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1f9e5c1d61c145b38d29b5dd563bf9c6
出典データセット
uspto-grants-2011_12
特許番号
US08076325B2

反応ノート

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