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Dicyclohexylcarbodiimide → 2,5-Pyrrolidinedione, 1-[[(2,6-dimethyl-1-piperidinyl)acetyl]oxy]-

HRID 2364931
ノート
印刷プレビュー

反応式

HRID 2364931 の反応式
Cl.[CH3:2][CH:3]1[CH2:8][CH2:7][CH2:6][CH:5]([CH3:9])[N:4]1[CH2:10][C:11]([OH:13])=[O:12].O[N:15]1[C:19](=[O:20])[CH2:18][CH2:17][C:16]1=[O:21].C1(N=C=NC2CCCCC2)CCCCC1>CN(C=O)C>[O:21]=[C:16]1[CH2:17][CH2:18][C:19](=[O:20])[N:15]1[O:12][C:11](=[O:13])[CH2:10][N:4]1[CH:3]([CH3:2])[CH2:8][CH2:7][CH2:6][CH:5]1[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 45790887HCID 45790887、化合物

生成物 1

HCID 111847332,5-Pyrrolidinedione, 1-[[(2,6-dimethyl-1-piperidinyl)acetyl]oxy]-

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4.15 g (20 mMol) (2,6-dimethyl-piperidin-1-yl)-acetic acid hydrochloride (6), in 50 ml DMF, was added to 2.3 g (20 mMol) N-hydroxysuccinimide and 8.1 g (40 mMol) dicyclohexylcarbodiimide. The reaction mixture was stirred for 16 h at RT. The residue was filtered and the filtrate was evaporated under vacuum to dryness. After dissolving the residue in CH2Cl2, the solution was washed with NaHCO3, dried (sodium sulphate) and the solvent evaporated. The compound was then recrystallised from diisopropylether (A-Kohle).

後処理

  1. filtrationThe residue was filtered
  2. customthe filtrate was evaporated under vacuum to dryness
  3. dissolutionAfter dissolving the residue in CH2Cl2
  4. washthe solution was washed with NaHCO3
  5. dry with materialdried (sodium sulphate)
  6. customthe solvent evaporated
  7. customThe compound was then recrystallised from diisopropylether (A-Kohle)

出典と根拠

ORDレコード
ord-349e8d589b1942019ff256b0e484ee08
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08697604B2

反応ノート

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