Citric Acid → HCID 58453106, 화합물

HRID 1422518

반응식

HRID 1422518 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 58453106HCID 58453106, 화합물수율 64%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c120433afb5e4c8eaa5b4d6d03b5e644
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08927458B2

연결된 노트

불러오는 중…