Trifluoroacetic anhydride → Benzoic acid, 4-[methyl(trifluoroacetyl)amino]-

HRID 982278

반응식

HRID 982278 반응식
[CH3:1][N:2]([C:9]1[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[CH:11][CH:10]=1)[C:3](=[O:8])[C:4]([F:7])([F:6])[F:5].F[C:19](F)(F)[C:20]([O:22][C:23](=[O:28])[C:24](F)(F)F)=[O:21].[CH3:31]NC1C=CC(C(O)=O)=CC=1>C(OCC)C>[CH:23]([O:28][CH:17]([CH3:16])[CH3:9])([CH3:31])[CH3:24].[C:20]([O:22][CH2:23][CH3:24])(=[O:21])[CH3:19].[CH3:1][N:2]([C:9]1[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[CH:11][CH:10]=1)[C:3](=[O:8])[C:4]([F:6])([F:5])[F:7]

참가 물질

6

반응물 3

HCID 9845Trifluoroacetic anhydrideHCID 663454-(Methylamino)benzoic acidHCID 10514620Benzoic acid, 4-[methyl(trifluoroacetyl)amino]-

생성물 2

HCID 10514620Benzoic acid, 4-[methyl(trifluoroacetyl)amino]-HCID 22281796Diisopropylether ethyl acetate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
0 °C

실험 절차

4-(N-Methyltrifluoroacetamido)benzoic acid may be prepared in the following manner: a solution of trifluoroacetic anhydride (43.75 g) in anhydrous diethyl ether (50 cc) is added to a solution of 4-methylaminobenzoic acid (21 g) in anhydrous diethyl ether (200 cc) while the temperature is maintained in the vicinity of 0° C. The reaction mixture is then stirred for 20 hours at a temperature in the region of 20° C. and is thereafter concentrated to dryness under reduced pressure (2.7 kPa). On recrystallization of the residue obtained in a diisopropyl ether/ethyl acetate mixture (80:20 by volume), 4-(N-methyltrifluoroacetamido)benzoic acid (7.5 g), m.p. 175° C., is obtained.

후처리

  1. concentrationis thereafter concentrated to dryness under reduced pressure (2.7 kPa)
  2. customOn recrystallization of the residue

출처 및 근거

ORD 기록
ord-a22dcb7959d248adbede47b43d95ab2f
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04994569

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