Dicyclohexylcarbodiimide → HCID 11253866、化合物

HRID 2364930ノート

反応式

HRID 2364930 の反応式
Cl.[CH:2]([N:5]([CH2:9][C:10]([OH:12])=[O:11])[CH:6]([CH3:8])[CH3:7])([CH3:4])[CH3:3].O[N:14]1[C:18](=[O:19])[CH2:17][CH2:16][C:15]1=[O:20].C1(N=C=NC2CCCCC2)CCCCC1>CN(C=O)C>[O:20]=[C:15]1[CH2:16][CH2:17][C:18](=[O:19])[N:14]1[O:11][C:10](=[O:12])[CH2:9][N:5]([CH:6]([CH3:7])[CH3:8])[CH:2]([CH3:3])[CH3:4]

参加物

5

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 46735981Diisopropylamino-acetic acid hydrochloride

生成物 1

HCID 11253866HCID 11253866、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3.82 g (19.5 mMol) diisopropylamino-acetic acid hydrochloride (3), in 50 ml DMF, was added to 2.24 g (19.5 mMol) N-hydroxysuccinimide and 8.04 g (39 nMol) dicyclohexylcarbodiimide. The reaction mixture was stirred for 16 h at RT. The residue was filtered and the filtrate was evaporated in 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.

後処理

  1. filtrationThe residue was filtered
  2. customthe filtrate was evaporated in 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

出典と根拠

ORDレコード
ord-e82303fbef3d496fbcc8564df4c013f7
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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