Diethyl Ether → HCID 67227223、化合物

HRID 573042

反応式

HRID 573042 の反応式
F[C:2]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5].[O-]P([O-])([O-])=O.[K+].[K+].[K+].[CH3:22][C:23]1[NH:24][C:25]2[C:30]([CH:31]=1)=[CH:29][C:28]([OH:32])=[CH:27][CH:26]=2.CCOCC>COCCOCCOC>[F:13][C:11]1[CH:10]=[CH:9][C:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])=[C:2]([O:32][C:28]2[CH:29]=[C:30]3[C:25](=[CH:26][CH:27]=2)[NH:24][C:23]([CH3:22])=[CH:31]3)[CH:12]=1

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 62657Potassium Phosphate, TribasicHCID 833362-methyl-1H-indol-5-olHCID 2737170Benzoic acid, 2,4-difluoro-, ethyl ester

生成物 1

HCID 67227223HCID 67227223、化合物

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

実験手順

Ethyl 2,4-difluorobenzoate (1.14 g), K3PO4 (1.30 g) and 2-methyl-5-indolol (0.90 g) were stirred at 110° C. in diglyme (12 mL) for 24 hours. The mixture was cooled and poured into ether. The solution was washed three times with 1M NaOH solution, and with brine, and dried. The solution was then concentrated. The concentrate was chromatographed on silica gel with 10% ethyl acetate/hexanes.

後処理

  1. temperatureThe mixture was cooled
  2. washThe solution was washed three times with 1M NaOH solution
  3. dry with materialwith brine, and dried
  4. concentrationThe solution was then concentrated
  5. customThe concentrate was chromatographed on silica gel with 10% ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-1ee6f62c08ad4d0db339638b3a8d1d3c
出典データセット
uspto-grants-2015_05
特許番号
US09029404B2

関連ノート

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