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

HRID 1168971ノート

反応式

HRID 1168971 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0c99a90a72ae4a358e6630840e034b41
出典データセット
uspto-grants-2003_09
特許番号
US06627648B1

反応ノート

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