Potassium Carbonate → 2,5-Difluoro-4-[4-chloro-3-(trifluoromethyl)phenylmethoxy]-benzonitrile

HRID 508446

반응식

HRID 508446 반응식
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][OH:7])=[CH:4][C:3]=1[C:10]([F:13])([F:12])[F:11].[F:14][C:15]1[CH:22]=[C:21](F)[C:20]([F:24])=[CH:19][C:16]=1[C:17]#[N:18].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[F:14][C:15]1[CH:22]=[C:21]([O:7][CH2:6][C:5]2[CH:8]=[CH:9][C:2]([Cl:1])=[C:3]([C:10]([F:11])([F:12])[F:13])[CH:4]=2)[C:20]([F:24])=[CH:19][C:16]=1[C:17]#[N:18]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 5938132,4,5-TrifluorobenzonitrileHCID 27781114-Chloro-3-(trifluoromethyl)benzyl alcohol

생성물 1

HCID 866825572,5-Difluoro-4-[4-chloro-3-(trifluoromethyl)phenylmethoxy]-benzonitrile수율 97%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of 4-chloro-3-(trifluoromethyl)-benzylalcohol (0.27 g, 1.28 mmol) and 2,4,5-trifluorobenzonitrile (0.2 g, 1.28 mmol) in DMSO (5 mL) was added potassium carbonate (0.33 g, 0.25 mmol). The resulting mixture was stirred at room temperature for 18 hours. The reaction mixture was partitioned between water (15 mL) and EtOAc (20 mL). The organic layer was separated, dried over magnesium sulphate, filtered and evaporated to yield the title compound (0.43 g, 97%).

후처리

  1. customThe reaction mixture was partitioned between water (15 mL) and EtOAc (20 mL)
  2. customThe organic layer was separated
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-97ecc8f7c6b84c2390c803a275b8b8e3
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096500B2

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