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

HRID 570089
ノート
印刷プレビュー

反応式

HRID 570089 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]>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

4

反応物 2

HCID 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

12.60 g (60 mMol) (2,6-Dimethyl-piperidin-1-yl)-acetic acid hydrochloride (5), in 100 ml DMF, was added to 7.02 g (60 mMol) N-hydroxysuccinimide and 12.58 g (60 mMol) N,N-dicyclohexylcarbodiimide. The reaction mixture was stirred for 16 h at RT. The residue was filtered and the filtrate was evaporated in vacuo to dryness. After dissolving the residue in 300 ml CH2Cl2, the solution was washed with NaHCO3, dried over sodium sulphate and the solvent was evaporated. The compound was then recrystallised from diisopropylether (activated charcoal).

後処理

  1. filtrationThe residue was filtered
  2. customthe filtrate was evaporated in vacuo to dryness
  3. dissolutionAfter dissolving the residue in 300 ml CH2Cl2
  4. washthe solution was washed with NaHCO3
  5. dry with materialdried over sodium sulphate
  6. customthe solvent was evaporated
  7. customThe compound was then recrystallised from diisopropylether (activated charcoal)

出典と根拠

ORDレコード
ord-88bdae61eb98419aa9d5aff4c9fe1234
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09023656B2

反応ノート

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