Dicyclohexylcarbodiimide → HCID 131731312、化合物

HRID 2364936ノート

反応式

HRID 2364936 の反応式
[CH3:1][N:2]([CH3:9])[CH:3]([CH3:8])[CH2:4][C:5]([OH:7])=[O:6].O[N:11]1[C:15](=[O:16])[CH2:14][CH2:13][C:12]1=[O:17].C1(N=C=NC2CCCCC2)CCCCC1.O.[C:34]1([CH3:44])[CH:39]=[CH:38][C:37]([S:40]([OH:43])(=[O:42])=[O:41])=[CH:36][CH:35]=1>C(Cl)Cl.C(#N)C>[S:40]([C:37]1[CH:38]=[CH:39][C:34]([CH3:44])=[CH:35][CH:36]=1)([OH:43])(=[O:42])=[O:41].[O:17]=[C:12]1[CH2:13][CH2:14][C:15](=[O:16])[N:11]1[O:6][C:5](=[O:7])[CH2:4][CH:3]([N:2]([CH3:9])[CH3:1])[CH3:8]

参加物

7

反応物 4

HCID 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 521998p-Toluenesulfonic acid monohydrateHCID 219359823-(Dimethylamino)butanoic acid

生成物 1

HCID 131731312HCID 131731312、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

6.55 g (50 mMol) 3-dimethylamino-butyric acid 20 was added to 5.75 g (50 mMol) N-hydroxysuccinimide and 11.05 g (55 mMol) dicyclohexyl carbodiimide in 100 ml CH2Cl2. The reaction mixture was stirred for 16 h at RT. The obtained urea was filtrated and the solution was evaporated. The residue, dissolved in 10 ml acetonitrile, was added under stirring to a solution of 9.51 g (50 mMol) 4-toluenesulfonic acid monohydrate in acetonitrile (30 ml). The solvent was evaporated under vacuum and the product was recrystallized from acetonitrile or acetone.

後処理

  1. filtrationThe obtained urea was filtrated
  2. customthe solution was evaporated
  3. dissolutionThe residue, dissolved in 10 ml acetonitrile
  4. additionwas added
  5. customThe solvent was evaporated under vacuum
  6. customthe product was recrystallized from acetonitrile or acetone

出典と根拠

ORDレコード
ord-c7059a9b925344ac8b10595ff68b7bbf
出典データセット
uspto-grants-2014_04
特許番号
US08697604B2

反応ノート

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