Water → HCID 12979370、化合物

HRID 492127

反応式

HRID 492127 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([CH2:11][C:12](=O)[CH3:13])[N:4]=1.Cl.[CH3:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[NH:23]N.C(OCC)(=O)C.O>C1(C)C=CC=CC=1.[Cl-].[Zn+2].[Cl-].C(OCC)(=O)C.CCCCCC>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([C:11]2[C:19]3[C:18](=[C:17]([CH3:16])[CH:22]=[CH:21][CH:20]=3)[NH:23][C:12]=2[CH3:13])[N:4]=1

参加物

8

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 71554o-Tolylhydrazinium(1+) chlorideHCID 112640521-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one

生成物 1

HCID 12979370HCID 12979370、化合物収率 34.2%

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒HCID 1140Toluene溶媒HCID 21226206Ethyl acetate hexane溶媒

実験手順

In 20 ml of toluene were dissolved 0.77 g (3.9 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone and 0.69 g (4.3 m moles) of 2-methylphenylhydrazine hydrochloride. Thereto was added 0.64 g (4.7 m moles) of zinc chloride, followed by refluxing for 2 hours. The reaction mixture was allowed to cool, and then ethyl acetate and water were added to dissolve the whole reaction mixture. The oily layer was washed with water, separated and dried over Glauber's salt. The resulting oily layer was concentrated under reduced pressure using a rotary evaporator, to obtain an orange solid. The solid was treated with ethyl acetate/n-hexane to obtain 0.38 g (1.34 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-2,7-dimethylindole. Yield: 34% Melting point: 145 to 147° C.

後処理

  1. temperatureby refluxing for 2 hours
  2. temperatureto cool
  3. dissolutionto dissolve
  4. customthe whole reaction mixture
  5. washThe oily layer was washed with water
  6. customseparated
  7. dry with materialdried over Glauber's salt
  8. concentrationThe resulting oily layer was concentrated under reduced pressure
  9. customa rotary evaporator
  10. customto obtain an orange solid

出典と根拠

ORDレコード
ord-cc58131cbc6b4fbbbc88843292773688
出典データセット
uspto-grants-2009_05
特許番号
US07531654B2

関連ノート

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