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

HRID 903131

반응식

HRID 903131 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-05ba8cda715a4cb3864f6eec80ea4e74
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04226861

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