Chlorodiphenylmethane → 1-(Diphenylmethyl)-1H-pyrazole-4-carboxylic acid ethyl ester

HRID 131633

반응식

HRID 131633 반응식
[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][NH:9][CH:10]=1)=[O:5])[CH3:2].[CH:11](Cl)([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>CN1CCCC1=O.O>[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:10]=1)=[O:5])[CH3:2]

참가 물질

6

반응물 3

HCID 7035ChlorodiphenylmethaneHCID 11430Potassium CarbonateHCID 142179ethyl 1H-pyrazole-4-carboxylate

생성물 1

HCID 693134381-(Diphenylmethyl)-1H-pyrazole-4-carboxylic acid ethyl ester

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
100 °C

실험 절차

A suspension of 1H-pyrazole-4-carboxylic acid ethyl ester (1.0 g), benzhydryl chloride (1.9 ml) and potassium carbonate (1.48 g) in anhydrous 1-methyl-2-pyrrolidinone (10 ml) was heated at 100° C. under nitrogen for 6 h. It was diluted with water and extracted with ethyl acetate, the organic extracts washed with water, dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by column chromatography over silica, eluting with i-hexane/ethyl acetate (4:1) followed by i-hexane/ethyl acetate (2:1) to give the sub-title compound (2.18 g).

후처리

  1. extractionextracted with ethyl acetate
  2. washthe organic extracts washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography over silica
  7. washeluting with i-hexane/ethyl acetate (4:1)

출처 및 근거

ORD 기록
ord-b9eb24beb22d458e8dd7dc49124f29a9
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07384951B2

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