Potassium Carbonate → (3-Amino-propyl)-methyl-carbamic acid isopropyl ester

HRID 870673ノート

反応式

HRID 870673 の反応式
[CH:1]([O:4][C:5](=[O:18])[N:6]([CH3:17])[CH2:7][CH2:8][CH2:9][NH:10]C(=O)C(F)(F)F)([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+]>CO.O>[CH:1]([O:4][C:5](=[O:18])[N:6]([CH2:7][CH2:8][CH2:9][NH2:10])[CH3:17])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 86696374Methyl-[3-(2,2,2-trifluoro-acetylamino)-propyl]-carbamic acid isopropyl ester

生成物 1

HCID 61799490(3-Amino-propyl)-methyl-carbamic acid isopropyl ester収率 109.1%

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

A suspension of methyl-[3-(2,2,2-trifluoro-acetylamino)-propyl]-carbamic acid isopropyl ester (9.0 g, 33.15 mmol), and potassium carbonate [584-08-7] in 50% (v/v) methanol/water (200 mL) was stirred at ambient temperature, under N2 blanket for 17 h, filtered, and the filtrate evaporated to reduce its volume. The resultant aqueous product solution was place in a continuous extractor and extracted with ethyl acetate to 2d. The ethyl acetate extract was dried (CaSO4) and evaporated to afford 6.3 g of clear yellow oil. LRMS (ESI) m/z 175.1 [(M+H)]+, calc'd for C8H18N2O2: 174.24.

後処理

  1. filtrationfiltered
  2. customthe filtrate evaporated
  3. extractionextracted with ethyl acetate to 2d
  4. extractionThe ethyl acetate extract
  5. dry with materialwas dried (CaSO4)
  6. customevaporated

出典と根拠

ORDレコード
ord-735979d8fea8492db74145ed2c54a2b0
出典データセット
uspto-grants-2015_03
特許番号
US08969565B2

反応ノート

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