Chloroacetic Acid → N,N-Diethylglycine

HRID 1516137

反応式

HRID 1516137 の反応式
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].Cl[CH2:7][C:8]([OH:10])=[O:9]>CC(OC)(C)C>[CH2:1]([N:3]([CH2:7][C:8]([OH:10])=[O:9])[CH2:4][CH3:5])[CH3:2]

参加物

4

反応物 2

HCID 300Chloroacetic AcidHCID 8021Diethylamine

生成物 1

HCID 74151N,N-Diethylglycine

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒

反応条件

温度
3 °C

実験手順

Diethylamine (9.5 L) was charged into a 20 L glass-lined reactor and cooled to 3° C. Chloroacetic acid (1.21 kg) in MTBE (1.8 L) was added over 1 hour with cooling—the temperature rose to 16° C. during the addition. The mixture was warmed to 20° C., stirred over night and concentrated on rotary evaporator giving yellow oil. This oil was re-concentrated with iPrOAc, mixed with iPrOAc (4.5 L) and stirred over night. The off-white hygroscopic precipitate was filtered, washed with iPrOAc (1.5 L) and immediately placed into a drying cabinet to avoid deliquescence. After drying, titled product was obtained (820 g, Y=49%).

後処理

  1. additionrose to 16° C. during the addition
  2. temperatureThe mixture was warmed to 20° C.
  3. concentrationconcentrated on rotary evaporator
  4. customgiving yellow oil
  5. concentrationThis oil was re-concentrated with iPrOAc
  6. additionmixed with iPrOAc (4.5 L)
  7. stirringstirred over night
  8. filtrationThe off-white hygroscopic precipitate was filtered
  9. washwashed with iPrOAc (1.5 L)
  10. customAfter drying

出典と根拠

ORDレコード
ord-27b689454e0a40369c14617ecde24831
出典データセット
uspto-grants-2012_07
特許番号
US08227428B2

関連ノート

読み込み中…