Water → (3-(5-Chloro(3-pyridyloxy))-1-methylpropyl)methylamine Hemigalactarate

HRID 1168971노트

반응식

HRID 1168971 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([O:8][CH2:9][CH2:10][CH:11]([NH:13][CH3:14])[CH3:12])[CH:5]=[N:6][CH:7]=1.[O:15]=[C:16]([OH:28])[C@@H:17]([C@H:19]([C@H:21]([C@@H:23]([C:25]([OH:27])=[O:26])[OH:24])[OH:22])[OH:20])[OH:18].O>C(O)C>[O:15]=[C:16]([OH:28])[C@@H:17]([C@H:19]([C@H:21]([C@@H:23]([C:25]([OH:27])=[O:26])[OH:24])[OH:22])[OH:20])[OH:18].[Cl:1][C:2]1[CH:3]=[C:4]([O:8][CH2:9][CH2:10][CH:11]([NH:13][CH3:14])[CH3:12])[CH:5]=[N:6][CH:7]=1.[Cl:1][C:2]1[CH:3]=[C:4]([O:8][CH2:9][CH2:10][CH:11]([NH:13][CH3:14])[CH3:12])[CH:5]=[N:6][CH:7]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 3037582Galactaric acidHCID 9942566(3-(5-Chloro(3-pyridyloxy))-1-methylpropyl)methylamine

생성물 1

HCID 131723464(3-(5-Chloro(3-pyridyloxy))-1-methylpropyl)methylamine Hemigalactarate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of (3-(5-chloro(3-pyridyloxy))-1-methylpropyl)methylamine (0.70 g, 3.27 mmol) in ethanol (20 mL) at 70° C. was added galactaric acid (0.343 g, 1.63 mmol). Water (0.5 mL) was added drop-wise while stirring, producing a clear solution. Some white, insoluble solids were removed by filtration. The filtrate was concentrated to 10 mL and was allowed to cool to ambient temperature. After standing 16 h, the precipitate was filtered, washed with ether (10 mL) and vacuum dried at 45° C. for 24 h to give 0.775 g (74.3%) of a light-beige, amorphous powder, mp 155-157° C. The compound exhibits a Ki of 1601 nM. The compound exhibits neurotransmitter release of 30 percent.

후처리

  1. customproducing a clear solution
  2. customSome white, insoluble solids were removed by filtration
  3. concentrationThe filtrate was concentrated to 10 mL
  4. filtrationthe precipitate was filtered
  5. washwashed with ether (10 mL) and vacuum
  6. customdried at 45° C. for 24 h
  7. customto give 0.775 g (74.3%) of a light-beige, amorphous powder, mp 155-157° C

출처 및 근거

ORD 기록
ord-0c99a90a72ae4a358e6630840e034b41
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06627648B1

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