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Potassium Carbonate → HCID 53963767, 화합물

HRID 1262786
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HRID 1262786 반응식
[F:1][C:2]1[CH:7]=[C:6](F)[CH:5]=[C:4]([CH3:9])[N:3]=1.[Cl:10][C:11]1[CH:16]=[C:15]([S:17][CH3:18])[C:14]([Cl:19])=[CH:13][C:12]=1[OH:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:1][C:2]1[CH:7]=[C:6]([O:20][C:12]2[CH:13]=[C:14]([Cl:19])[C:15]([S:17][CH3:18])=[CH:16][C:11]=2[Cl:10])[CH:5]=[C:4]([CH3:9])[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 204558722,4-Difluoro-6-methylpyridineHCID 54506707HCID 54506707, 화합물

생성물 1

HCID 53963767HCID 53963767, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Amounts of 12.9 gm (0.1 mol) of 2,4-difluoro-6-methylpyridine, 20.7 gm (0.1 mol) of 2,5-dichloro-4-methylmercaptophenol, and 13.8 gm (0.1 mol) of potassium carbonate in 100 ml of dimethylformamide were stirred for 10 hours at 100° C. The resulting solution was then poured onto 500 ml of ice water, and the precipitate formed was recovered by suction filtration and washed with water. It was then taken up in methylene chloride, and this solution was dried over sodium sulphate and evaporated down. The oil obtained was purified over a silica gel column (ethylene chloride as the eluant) and 16.3 gm (57% of theory) of the desired ether were obtained.

후처리

  1. customthe precipitate formed
  2. filtrationwas recovered by suction filtration
  3. washwashed with water
  4. dry with materialthis solution was dried over sodium sulphate
  5. customevaporated down
  6. customThe oil obtained
  7. customwas purified over a silica gel column (ethylene chloride as the eluant) and 16.3 gm (57% of theory) of the desired ether
  8. customwere obtained

출처 및 근거

ORD 기록
ord-ca585409c82f41a389797aa20e92f202
출처 데이터셋
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04453972

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