Methyl iodide → HCID 15790490, 화합물

HRID 2253797노트

반응식

HRID 2253797 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]([OH:15])[CH:10]=[CH:11][C:12]=2[C:13]#[N:14])=[CH:4][CH:3]=1.O1CCC[CH2:17]1.CC(C)([O-])C.[K+].CI>O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]([O:15][CH3:17])[CH:10]=[CH:11][C:12]=2[C:13]#[N:14])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 8028TetrahydrofuranHCID 157904882-(4-Chlorophenyl)-1-hydroxy-1H-pyrrole-3-carbonitrileHCID 23665647Potassium tert-butoxide

생성물 1

HCID 15790490HCID 15790490, 화합물수율 77%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred solution of 2-(p-chlorophenyl)-1-hydroxypyrrole-3-carbonitrile (2.88 g, 0.0132 mol) and anhydrous tetrahydrofuran is added potassium tert-butoxide (1.55 g, 0.0138 mol). After 30 minutes, methyl iodide (2.06 g, 0.9 mL, 0.0145 mol) is added and the resulting slurry is stirred at room temperature for 3 hours, diluted with water and extracted with ether. The combined ether extracts are washed sequentially with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to yield a solid. Crystallization of the solid from ether/hexanes gives the title compound as a brown solid (2.35 g, 77%), mp 105°-106° C.

후처리

  1. extractionextracted with ether
  2. washThe combined ether extracts are washed sequentially with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customto yield a solid
  6. customCrystallization of the solid from ether/hexanes

출처 및 근거

ORD 기록
ord-c9ac1c7bcb004f2da6952ad2775d7b5a
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05232979

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