Citric Acid → HCID 58453106、化合物

HRID 1422518

反応式

HRID 1422518 の反応式
[H-].[Na+].[CH:3]1([C:6](=[O:10])[CH2:7][C:8]#[N:9])[CH2:5][CH2:4]1.[CH3:11][C:12]1[N:20]=[C:19]([N:21]2[CH:25]=[N:24][CH:23]=[N:22]2)[CH:18]=[CH:17][C:13]=1[C:14](Cl)=[O:15].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>C1COCC1>[CH:3]1([C:6](=[O:10])[CH:7]([C:14]([C:13]2[C:12]([CH3:11])=[N:20][C:19]([N:21]3[CH:25]=[N:24][CH:23]=[N:22]3)=[CH:18][CH:17]=2)=[O:15])[C:8]#[N:9])[CH2:5][CH2:4]1

参加物

6

反応物 4

HCID 311Citric AcidHCID 24758Sodium hydrideHCID 98127633-Cyclopropyl-3-oxopropanenitrileHCID 584530902-methyl-6-(1H-1,2,4-triazol-1-yl)nicotinic acid chloride

生成物 1

HCID 58453106HCID 58453106、化合物収率 64%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

A THF (2 ml) suspension of sodium hydride (0.06 g, 60% oil suspension, 18.78 mmol) was cooled in an ice bath, and a THF (2 ml) solution of 3-cyclopropyl-3-oxopropanenitrile was dripped thereto. To the obtained reaction solution, a THF (3 ml) solution of 2-methyl-6-(1H-1,2,4-triazol-1-yl)nicotinic acid chloride (0.16 g, 0.73 mmol) was dripped. The resultant was stirred at room temperature for 3 hours. The obtained reaction solution was made acidic with a citric acid aqueous solution, and the product was extracted with ethyl acetate. The obtained organic layer was washed with water, dried with magnesium sulfate and concentrated to obtain the desired product (0.14 g, yield 64%).

後処理

  1. temperaturewas cooled in an ice bath
  2. customTo the obtained reaction solution
  3. customThe obtained reaction solution
  4. extractionthe product was extracted with ethyl acetate
  5. washThe obtained organic layer was washed with water
  6. dry with materialdried with magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-c120433afb5e4c8eaa5b4d6d03b5e644
出典データセット
uspto-grants-2015_01
特許番号
US08927458B2

関連ノート

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