Water → Calcium 3-(4,6-dimethoxypyrimidin-2-yl)oxy-6-dimethylaminopicolinate

HRID 274879ノート

反応式

HRID 274879 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([O:11][C:12]2[C:13]([C:21]([O-:23])=[O:22])=[N:14][C:15]([N:18]([CH3:20])[CH3:19])=[CH:16][CH:17]=2)[N:4]=1.[K+].C(=O)([O-])[O-].[Ca+2:29].O>O1CCCC1>[CH3:10][O:9][C:7]1[CH:8]=[C:3]([O:2][CH3:1])[N:4]=[C:5]([O:11][C:12]2[C:13]([C:21]([O-:23])=[O:22])=[N:14][C:15]([N:18]([CH3:19])[CH3:20])=[CH:16][CH:17]=2)[N:6]=1.[Ca+2:29].[CH3:10][O:9][C:7]1[CH:8]=[C:3]([O:2][CH3:1])[N:4]=[C:5]([O:11][C:12]2[C:13]([C:21]([O-:23])=[O:22])=[N:14][C:15]([N:18]([CH3:19])[CH3:20])=[CH:16][CH:17]=2)[N:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 10112Calcium CarbonateHCID 23710069Potassium 3-(4,6-dimethoxypyrimidin-2-yl)oxy-6-dimethylaminopicolinate

生成物 1

HCID 23221890Calcium 3-(4,6-dimethoxypyrimidin-2-yl)oxy-6-dimethylaminopicolinate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1.0 g (3.1 mmol) of potassium 3-(4,6-dimethoxypyrimidin-2-yl)oxy-6-dimethylaminopicolinate was dissolved in 10 ml of tetrahydrofuran, and 0.15 g (1.5 mmol) of precipitated calcium carbonate was added thereto. Furthermore, 10 ml of water was added to the resultant mixture, and the mixture was stirred at room temperature. The reaction liquor was concentrated under reduced pressure, and acetone was added thereto to precipitate a crystal. The crystal thus obtained was separated by filtration and was washed with hexane to obtain an aimed compound.

後処理

  1. concentrationThe reaction liquor was concentrated under reduced pressure, and acetone
  2. additionwas added
  3. customto precipitate a crystal
  4. customThe crystal thus obtained
  5. customwas separated by filtration
  6. washwas washed with hexane

出典と根拠

ORDレコード
ord-88201f79872b4fd9a82dc9ab8aab7ed7
出典データセット
uspto-grants-1995_02
特許番号
US05391537

反応ノート

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