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

HRID 870673노트

반응식

HRID 870673 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-735979d8fea8492db74145ed2c54a2b0
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969565B2

반응 노트

불러오는 중…