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

HRID 508446

反応式

HRID 508446 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-97ecc8f7c6b84c2390c803a275b8b8e3
出典データセット
uspto-grants-2015_08
特許番号
US09096500B2

関連ノート

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