HCID 53629158、化合物 → HCID 178439462、化合物

HRID 1926767ノート

反応式

HRID 1926767 の反応式
[CH2:1]([CH:4]1[CH2:8][N:7]([CH2:9][C:10]2[N:11]=[CH:12][N:13](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:14]=2)[C:6](=[O:34])[CH2:5]1)[CH2:2][CH3:3]>CC(O)=O.O>[NH:13]1[CH:14]=[C:10]([CH2:9][N:7]2[CH2:8][CH:4]([CH2:1][CH2:2][CH3:3])[CH2:5][C:6]2=[O:34])[N:11]=[CH:12]1

参加物

3

反応物 1

HCID 53629158HCID 53629158、化合物

生成物 1

HCID 178439462HCID 178439462、化合物収率 88%

試薬・触媒・溶媒 1

HCID 21899381Acetic acid--water (1/1)溶媒

実験手順

In a 50 ml reaction flask fitted with a magnetic stirrer, 4-propyl-1-[(1-trityl-1H-imidazol-4-yl)methyl]pyrrolidin-2-one x45 (1.8 g, 4 mmol) is dissolved in a 1/1 mixture of CH3CO2H/H2O (30 ml) and the solution is stirred for 36 h at room temperature. Most of the solvents are removed under vacuum and the residue is dissolved in 1N HCl and diluted with CH2Cl2. The first organic phase is removed and pH of the aqueous phase is adjusted to 9 by addition of solid Na2CO3. Then CH2Cl2 is added and the second organic phase is separated, dried over MgSO4 and concentrated to dryness, affording 730 mg of 1-(1H-imidazol-4-ylmethyl)-4-propylpyrrolidin-2-one 110.

後処理

  1. customIn a 50 ml reaction flask
  2. customfitted with a magnetic stirrer
  3. customMost of the solvents are removed under vacuum
  4. dissolutionthe residue is dissolved in 1N HCl
  5. additiondiluted with CH2Cl2
  6. customThe first organic phase is removed
  7. additionpH of the aqueous phase is adjusted to 9 by addition of solid Na2CO3
  8. additionThen CH2Cl2 is added
  9. customthe second organic phase is separated
  10. dry with materialdried over MgSO4
  11. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-0ff7652bc0dd47f18ab822f0d0cbd9b3
出典データセット
uspto-grants-2012_05
特許番号
US08183241B2

反応ノート

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