Acetic Acid → N-Acetyl-L-proline

HRID 538952

反応式

HRID 538952 の反応式
[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]

参加物

3

反応物 2

HCID 176Acetic AcidHCID 145742L-Proline

生成物 1

HCID 66141N-Acetyl-L-proline収率 82.5%

反応条件

温度
150 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6ed644f87871434daf97c199c235ef07
出典データセット
uspto-grants-2014_10
特許番号
US08865920B2

関連ノート

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