Trifluoroacetic acid → (3S)-3-Amino-4,4-dimethylpentan-2-one

HRID 2084547노트

반응식

HRID 2084547 반응식
C(OC(=O)[NH:7][C@H:8]([C:13](=[O:15])[CH3:14])[C:9]([CH3:12])([CH3:11])[CH3:10])(C)(C)C.FC(F)(F)C(O)=O>ClCCl.CO>[NH2:7][C@@H:8]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:13](=[O:15])[CH3:14]

참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acidHCID 21305239(1(S)-Acetyl-2,2-dimethylpropyl)carbamic Acid-tert-butyl Ester

생성물 1

HCID 21305288(3S)-3-Amino-4,4-dimethylpentan-2-one수율 303.5%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

To a solution of (1(S)-acetyl-2,2-dimethylpropyl)carbamic acid-tert-butyl ester (700 mg, 2.55 mmol) in dichloromethane (10 mL) at 0° C. was added trifluoroacetic acid (5 mL). The reaction was left at <5° C. for 16 hours before the solvents were removed in vacuo to give a bright yellow oil. The residue was dissolved in methanol (30 mL) and was treated portionwise with Dowex 1X8-400 basic resin until pH 9. Filtration and removal of the solvents in vacuo gave the title compound as a pale yellow oil (˜1.0 g, >100%, residual water). The material was used without further purification.

후처리

  1. customwere removed in vacuo
  2. customto give a bright yellow oil
  3. additionwas treated portionwise with Dowex 1X8-400 basic resin until pH 9
  4. filtrationFiltration and removal of the solvents in vacuo

출처 및 근거

ORD 기록
ord-872bafbceae144b49a8f6de31ccf3ac3
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06716878B1

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