Trifluoroacetic acid → 2-(2,6-Diethylphenyl)-5-[(5-isopropyl-2-methylphenoxy)methyl]-4-methyl-6-piperazin-1-ylpyrimidine

HRID 1091941

反応式

HRID 1091941 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9][CH3:10])[C:4]=1[C:11]1[N:16]=[C:15]([N:17]2[CH2:22][CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18]2)[C:14]([CH2:30][O:31][C:32]2[CH:37]=[C:36]([CH:38]([CH3:40])[CH3:39])[CH:35]=[CH:34][C:33]=2[CH3:41])=[C:13]([CH3:42])[N:12]=1)[CH3:2].FC(F)(F)C(O)=O>C1(C)C=CC=CC=1>[CH2:9]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([CH2:1][CH3:2])[C:4]=1[C:11]1[N:12]=[C:13]([CH3:42])[C:14]([CH2:30][O:31][C:32]2[CH:37]=[C:36]([CH:38]([CH3:39])[CH3:40])[CH:35]=[CH:34][C:33]=2[CH3:41])=[C:15]([N:17]2[CH2:18][CH2:19][NH:20][CH2:21][CH2:22]2)[N:16]=1)[CH3:10]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 11548705Tert-butyl 4-{2-(2,6-diethylphenyl)-5-[(5-isopropyl-2-methylphenoxy)methyl]-6-methylpyrimidin-4-yl}piperazine-1-carboxylate

生成物 1

HCID 575314682-(2,6-Diethylphenyl)-5-[(5-isopropyl-2-methylphenoxy)methyl]-4-methyl-6-piperazin-1-ylpyrimidine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To tert-butyl 4-{2-(2,6-diethylphenyl)-5-[(5-isopropyl-2-methylphenoxy)methyl]-6-methylpyrimidin-4-yl}piperazine-1-carboxylate (228 mg, 0.40 mmol) is added trifluoroacetic acid (2 mL). Gas evolution ensues and rapidly subsides. Toluene (10 mL) is added and removed under reduced pressure. The resulting residue is dissolved in EtOAc (25 mL) and extracted with saturated potassium carbonate (10 mL) followed by brine (10 mL), dried over sodium sulfate, filtered and evaporated at reduced pressure to obtain the title compound as a colorless oil. LC/MS (Method 3), M+H=473.2, Rt=2.35 min.; 1H NMR (CDCl3) δ=7.26 (d, 1H), 7.12 (d, 3H), 6.83 (me, 2H), 4.99 (s, 2H), 3.49 (m, 8H), 2.91 (m, 1H), 2.56, (s, 3H), 2.42 (q, 4H) 2.24 (s, 3H), 1.42 (s, 9H), 1.28 (d, 6H), 1.13 (t, 6H).

後処理

  1. customremoved under reduced pressure
  2. dissolutionThe resulting residue is dissolved in EtOAc (25 mL)
  3. extractionextracted with saturated potassium carbonate (10 mL)
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated at reduced pressure

出典と根拠

ORDレコード
ord-7e69ad1ce4914885941cdd8510c789ee
出典データセット
uspto-grants-2012_03
特許番号
US08129395B2

関連ノート

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