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Methyl iodide → HCID 15581183, 화합물

HRID 1283127
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HRID 1283127 반응식
[Na].[N:2]1[CH:7]=[CH:6][CH:5]=[C:4]2[CH2:8][C:9]3[CH:15]=[C:14]([CH:16]([C:20]#[N:21])[C:17]([CH3:19])=[O:18])[CH:13]=[CH:12][C:10]=3[O:11][C:3]=12.[CH3:22]I>CN(C)C=O>[N:2]1[CH:7]=[CH:6][CH:5]=[C:4]2[CH2:8][C:9]3[CH:15]=[C:14]([C:16]([C:20]#[N:21])([CH3:22])[C:17](=[O:18])[CH3:19])[CH:13]=[CH:12][C:10]=3[O:11][C:3]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 5360545SodiumHCID 13066472HCID 13066472, 화합물

생성물 1

HCID 15581183HCID 15581183, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2.9 g of sodium salt of 1-(5H-[1]benzopyrano[2,3-b]pyridin-7-yl)-1-cyano-acetone is dissolved in 15 ml of dried dimethylformamide, 1.6 g of methyl iodide is added to the solution with stirring, and the mixture is stirred at room temperature for 1.5 hours. The reaction mixture is concentrated, and water is added to the oily residue. The crystalline precipitate is filtered off and recrystallized from ethanol to give 2.2 g of 3-(5H-[1]-benzopyrano[2,3-b]pyridin-7-yl)-3-cyano-2-butanone as white needles melting at 163.5°-164.5°C.

후처리

  1. stirringthe mixture is stirred at room temperature for 1.5 hours
  2. concentrationThe reaction mixture is concentrated
  3. additionwater is added to the oily residue
  4. filtrationThe crystalline precipitate is filtered off
  5. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-1ab0cf009b7044e1a84d958dd91798ba
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03974168

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