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

HRID 1350596

반응식

HRID 1350596 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 167264233-(N-Methylpentylamino)propionic acid hydrochloride수율 82.7%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
24 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-744adb86bb3e4a93923a6ff91260a4e5
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07214818B2

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