Acetic Acid → N-Acetyl-L-proline

HRID 538952

반응식

HRID 538952 반응식
[NH:1]1[CH2:8][CH2:7][CH2:6][C@H:2]1[C:3]([OH:5])=[O:4].[C:9](O)(=[O:11])[CH3:10]>>[C:9]([N:1]1[CH2:8][CH2:7][CH2:6][C@H:2]1[C:3]([OH:5])=[O:4])(=[O:11])[CH3:10]

참가 물질

3

반응물 2

HCID 176Acetic AcidHCID 145742L-Proline

생성물 1

HCID 66141N-Acetyl-L-proline수율 82.5%

반응 조건

온도
150 °C

실험 절차

Proline (1 g, 8.68 mmol) and acetic acid (20 mL) were mixed together and heated at 150° C. in a microwave for two hours. The excess acetic acid was removed using a rotary evaporator. The residue was stirred in MTBE at ambient temperature until a solid precipitated. The mixture was filtered and the solid was washed with MTBE. The solid was dried in a vacuum oven at 60° C. The product was obtained as a white solid (1.12 g, 82.5%). 1H NMR (500 MHz, DMSO-d6) δ ppm 1.77-1.95 (m, 4H), 1.97 (s, 2H), 2.0-2.19 (m, 1H), 3.35 (dt, 1H), 3.41-3.58 (m, 2H), 4.19 (dd, 1H).

후처리

  1. customThe excess acetic acid was removed
  2. customa rotary evaporator
  3. customprecipitated
  4. filtrationThe mixture was filtered
  5. washthe solid was washed with MTBE
  6. customThe solid was dried in a vacuum oven at 60° C

출처 및 근거

ORD 기록
ord-6ed644f87871434daf97c199c235ef07
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865920B2

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