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

HRID 650928ノート

反応式

HRID 650928 の反応式
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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 1140Toluene溶媒HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a21c3b9c151343858ede89557582c309
出典データセット
uspto-grants-2001_08
特許番号
US06277853B1

反応ノート

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