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

HRID 274879

반응식

HRID 274879 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-88201f79872b4fd9a82dc9ab8aab7ed7
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05391537

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