Trifluoroacetic acid → 4-[4-(4,5-Dihydrooxazol-2-yl)phenyl]piperazine

HRID 650928노트

반응식

HRID 650928 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([C:20]3[O:21][CH2:22][CH2:23][N:24]=3)=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C1(C)C=CC=CC=1.CO.C(N(CC)CC)C>[O:21]1[CH2:22][CH2:23][N:24]=[C:20]1[C:17]1[CH:18]=[CH:19][C:14]([N:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[CH:15][CH:16]=1

참가 물질

6

반응물 2

HCID 6422Trifluoroacetic acidHCID 18504842n-Tert-butoxycarbonyl-4-[4-(4,5-dihydrooxazol-2-yl)phenyl]piperazine

생성물 1

HCID 185048344-[4-(4,5-Dihydrooxazol-2-yl)phenyl]piperazine

시약·촉매·용매 3

HCID 887Methanol용매HCID 1140Toluene용매HCID 8471Triethylamine용매

실험 절차

Compound 5A (826 mg; 2.49 mmol) in solution in toluene (20 ml) is treated, at room temperature, with trifluoroacetic acid (2.75 ml). After 1 h, the medium is evaporated to dryness and coevaporated 3 times with toluene. The product obtained is taken up in methanol (20 ml) and triethylamine (8 ml), stirred for 15 min at room temperature and finally evaporated to dryness. The solid obtained is purified by chromatography on a silica gel column eluted with a dichloro-methane/methanol/ammonium hydroxide mixture in the proportions 90/9/1 to give the intermediate 5B.

후처리

  1. customthe medium is evaporated to dryness
  2. customThe product obtained
  3. customfinally evaporated to dryness
  4. customThe solid obtained
  5. customis purified by chromatography on a silica gel column
  6. washeluted with a dichloro-methane/methanol/ammonium hydroxide mixture in the proportions 90/9/1

출처 및 근거

ORD 기록
ord-a21c3b9c151343858ede89557582c309
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06277853B1

반응 노트

불러오는 중…