Dicyclohexylcarbodiimide → HCID 131731312, 화합물

HRID 2364936노트

반응식

HRID 2364936 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 131731312HCID 131731312, 화합물

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c7059a9b925344ac8b10595ff68b7bbf
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697604B2

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