Hydrochloric Acid → Benzyl 2-methyl-1-oxo-1-(2-oxoethylamino)propan-2-ylcarbamate

HRID 631961노트

반응식

HRID 631961 반응식
C[O:2][CH:3](OC)[CH2:4][NH:5][C:6](=[O:21])[C:7]([NH:10][C:11](=[O:20])[O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([CH3:9])[CH3:8].Cl.C(OCC)(=O)C>C1COCC1>[CH3:9][C:7]([NH:10][C:11](=[O:20])[O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([CH3:8])[C:6](=[O:21])[NH:5][CH2:4][CH:3]=[O:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 86674736Benzyl 1-(2,2-dimethoxyethylamino)-2-methyl-1-oxopropan-2-ylcarbamate

생성물 1

HCID 86674737Benzyl 2-methyl-1-oxo-1-(2-oxoethylamino)propan-2-ylcarbamate수율 100%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of benzyl 1-(2,2-dimethoxyethylamino)-2-methyl-1-oxopropan-2-ylcarbamate (0.52 g, 1.6 mmol) in THF (20 mL) was added 5 M hydrochloric acid (10 mL) and the mixture was stirred at room temperature until TLC showed the reaction was completed. Ethyl acetate (50 mL) was added and the phases were separated. The organic layer was washed with brine (4×30 mL) to pH=6-7, dried over anhydrous sodium sulfate and concentrated to yield product (0.445 g, 100%) as yellow oil, which was used directly in the next step without purification; MS: m/e 279.1 [M+H]+.

후처리

  1. customthe phases were separated
  2. washThe organic layer was washed with brine (4×30 mL) to pH=6-7
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-043b4af4100e47429abbd73e3f2a3e34
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321727B2

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