Cesium fluoride → HCID 89350931、化合物

HRID 1497314ノート

反応式

HRID 1497314 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:11]=2[F:17])[CH:5]=[C:4]([Cl:18])[N:3]=1.[F:19][C:20]([F:31])([F:30])[C:21]1[CH:22]=[C:23](B(O)O)[CH:24]=[N:25][CH:26]=1.[F-].[Cs+]>O1CCOCC1.O>[Cl:18][C:4]1[N:3]=[C:2]([C:23]2[CH:24]=[N:25][CH:26]=[C:21]([C:20]([F:31])([F:30])[F:19])[CH:22]=2)[N:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:11]=2[F:17])[CH:5]=1

参加物

5

反応物 3

HCID 25953Cesium fluorideHCID 45158900[5-(Trifluoromethyl)pyridin-3-yl]boronic acidHCID 89350889(2,6-Dichloro-pyrimidin-4-yl)-(2,4-difluoro-benzyl)-amine

生成物 1

HCID 89350931HCID 89350931、化合物

試薬・触媒・溶媒 1

HCID 218864351,4-Dioxane--water (1/1)溶媒

反応条件

温度
60 °C

実験手順

A mixture of (2,6-Dichloro-pyrimidin-4-yl)-(2,4-difluoro-benzyl)-amine (1 g, 0.0034 mol) and 5-trifluoromethylpyridine-3-boronic acid (0.726 g, 0.0038 mol) were taken in dioxane:water (20:5) ml and to this CsF (2.1 g, 0.0138 mol) was added and degassed. Then bis-triphenylphosphine-palladium(II) chloride (0.24 g, 0.00034 mol) was added and degassed. The mixture was stirred at 60° C. for 12 hrs. The reaction was cooled to room temperature diluted with water (50 ml) and ethyl acetate (100 ml). After standard work-up, the residue was purified by column chromatography to get compound as white solid.

後処理

  1. customdegassed
  2. customdegassed
  3. temperatureThe reaction was cooled to room temperature
  4. additiondiluted with water (50 ml) and ethyl acetate (100 ml)
  5. customAfter standard work-up, the residue was purified by column chromatography
  6. customto get compound as white solid

出典と根拠

ORDレコード
ord-5f6a859c98cb4b198eebfdd35b5928bc
出典データセット
uspto-grants-2015_12
特許番号
US09199962B2

反応ノート

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