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

HRID 631961ノート

反応式

HRID 631961 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-043b4af4100e47429abbd73e3f2a3e34
出典データセット
uspto-grants-2016_04
特許番号
US09321727B2

反応ノート

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