Hydrochloric Acid → 3-(N-Methylpentylamino)propionic acid hydrochloride

HRID 1350596

反応式

HRID 1350596 の反応式
C[O:2][C:3](=[O:13])[CH2:4][CH2:5][N:6]([CH3:12])[CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[ClH:14]>O>[ClH:14].[CH3:12][N:6]([CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])[CH2:5][CH2:4][C:3]([OH:13])=[O:2]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 16726422Methyl 3-(methyl(pentyl)amino)propanoate

生成物 1

HCID 167264233-(N-Methylpentylamino)propionic acid hydrochloride収率 82.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
24 °C

実験手順

68.8 g (367.4 mmol) N-methyl-N-pentyl-β-alanine methyl ester was hydrolyzed by refluxing with 138 ml water. Then the water is partly distilled off and 83 ml (472.7 mmol) hydrochloric acid (19%) was added. Water was distilled off again and 230 ml methyl ethyl ketone was added to remove residual water by azeotropic distillation. The reaction mixture was then cooled to 24° C. The crystallized product was separated and washed with methyl ethyl ketone and subsequently dried in vacuo. 63.7 g (82.7%) N-methyl-N-pentyl-β-alanine hydrochloride were obtained.

後処理

  1. distillationThen the water is partly distilled off
  2. distillationWater was distilled off again
  3. addition230 ml methyl ethyl ketone was added
  4. customto remove residual water
  5. distillationby azeotropic distillation
  6. customThe crystallized product was separated
  7. washwashed with methyl ethyl ketone
  8. customsubsequently dried in vacuo

出典と根拠

ORDレコード
ord-744adb86bb3e4a93923a6ff91260a4e5
出典データセット
uspto-grants-2007_05
特許番号
US07214818B2

関連ノート

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