Oxalic Acid → 3-(4-Trifluoromethylphenoxy)-N-methyl-1-azetidinecarboxamide

HRID 903131

反応式

HRID 903131 の反応式
C(O)(=O)C(O)=O.[F:7][C:8]([F:21])([F:20])[C:9]1[CH:19]=[CH:18][C:12]([O:13][CH:14]2[CH2:17][NH:16][CH2:15]2)=[CH:11][CH:10]=1.[OH-].[K+].[CH3:24][N:25]=[C:26]=[O:27]>C1C=CC=CC=1>[CH3:24][NH:25][C:26]([N:16]1[CH2:15][CH:14]([O:13][C:12]2[CH:11]=[CH:10][C:9]([C:8]([F:7])([F:20])[F:21])=[CH:19][CH:18]=2)[CH2:17]1)=[O:27]

参加物

6

反応物 4

HCID 971Oxalic AcidHCID 12228Methyl IsocyanateHCID 14797Potassium HydroxideHCID 128124993-[4-(Trifluoromethyl)phenoxy]azetidine

生成物 1

HCID 134201663-(4-Trifluoromethylphenoxy)-N-methyl-1-azetidinecarboxamide

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

The oxalic acid salt of 3-(4-trifluoromethylphenoxy) azetidine (13.0 g., 0.042 mole) was partitioned between 50 ml. of benzene and 50 ml. of potassium hydroxide solution. The benzene layer was dried over calcium sulfate and filtered, and to the stirring dried benzene solution was added 2.6 g. (0.046 mole) of methyl-isocyanate. Stirring was continued overnight. The mixture was concentrated at reduced pressure and the solid residue was recrystallized from a mixture of isopropyl ether-ethyl acetate. The product weighed 7.5 g. (65%) and melted at 154°-157° C.

後処理

  1. dry with materialThe benzene layer was dried over calcium sulfate
  2. filtrationfiltered
  3. additionto the stirring dried benzene solution was added 2.6 g
  4. concentrationThe mixture was concentrated at reduced pressure
  5. customthe solid residue was recrystallized from a mixture of isopropyl ether-ethyl acetate

出典と根拠

ORDレコード
ord-05ba8cda715a4cb3864f6eec80ea4e74
出典データセット
uspto-grants-1980_10
特許番号
US04226861

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