Trifluoroacetic acid → HCID 68512974、化合物

HRID 1716268ノート

反応式

HRID 1716268 の反応式
C(OC(=O)[NH:7][C@@H:8]1[CH2:14][CH:13]=[CH:12][CH2:11][N:10]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]1=[O:23])(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[NH2:7][C@@H:8]1[CH2:14][CH:13]=[CH:12][CH2:11][N:10]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]1=[O:23]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 68514761(1-benzyloxy-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-(R)-yl)-carbamic acid tert-butyl ester

生成物 1

HCID 68512974HCID 68512974、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4.14 g (12.45 mmoles) of (1-benzyloxy-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-(R)-yl)-carbamic acid tert-butyl ester from Step C in 30 mL of dichloromethane was added 20 mL of trifluoroacetic acid. The reaction mixture was stirred for two hours at room temperature, and the solvent was removed under vacuum. Next, the reaction mixture was diluted in dichloromethane, and neutralized with NaHCO3(s). The reaction mixture was then extracted with NaHCO3(aq.) and NaCl (aq.) solutions. The aqueous layers were re-extracted with dichloromethane twice, and the organic layers combined and dried over Na2SO4(s). Filtration and solvent removal gave 3.685 g of a purple, viscous oil. MS: 465 (2M+H), 233 (M+H).

後処理

  1. customthe solvent was removed under vacuum
  2. additionNext, the reaction mixture was diluted in dichloromethane
  3. extractionThe reaction mixture was then extracted with NaHCO3(aq.) and NaCl (aq.) solutions
  4. extractionThe aqueous layers were re-extracted with dichloromethane twice
  5. dry with materialdried over Na2SO4(s)
  6. filtrationFiltration and solvent removal
  7. customgave 3.685 g of a purple, viscous oil

出典と根拠

ORDレコード
ord-844f4b9d7272457f953544733d0bb126
出典データセット
uspto-grants-2010_09
特許番号
US07803793B2

反応ノート

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