Dicyclohexylcarbodiimide → HCID 86747153、化合物

HRID 2255163ノート

反応式

HRID 2255163 の反応式
[NH2:1][CH:2]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[C:3]([O:5][CH2:6][CH3:7])=[O:4].O[CH:14]([CH2:18][CH:19]([CH3:21])[CH3:20])[C:15](O)=[O:16].[OH:22][N:23]1C(=O)CCC1=O.C1(N=C=NC2CCCCC2)CCCCC1>O1CCOCC1>[OH:22][N:23]=[C:14]([CH2:18][CH:19]([CH3:21])[CH3:20])[C:15]([NH:1][CH:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])[C:8]([O:10][CH2:11][CH3:12])=[O:9])=[O:16]

参加物

6

反応物 4

HCID 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 81272Propanedioic acid, 2-amino-, 1,3-diethyl ester2 回HCID 92779(+-)-2-Hydroxyisocaproic acid

生成物 1

HCID 86747153HCID 86747153、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

30 Milliliters of water and 7.0 g of sodium hydrogen carbonate were added to a suspension of 17.5 g of diethyl aminomalonate hydrochloride in 150 ml of dichloromethane. After 20 minutes, the dichloromethane layer was separated and dried over magnesium sulfate. The solvent was removed by evaporation under reduced pressure to obtain colorless oily diethyl aminomalonate. The diethyl aminomalonate was made into a solution of the diethyl aminomalonate, 10.0 g of α-hydroxyisocaproic acid and 8.7 g of N-hydroxysuccinimide dissolved in 200 ml of dioxane. To the solution was added 15.7 g of N,N'-dicyclohexylcarbodiimide. The mixture was stirred for 16 hours at room temperature and then filtered. The filtrate was subjected to removal of the solvent by evaporation. The residue was mixed with ethyl acetate, and the mixture was washed with 10% hydrochloric acid, water, an aqueous solution saturated with sodium hydrogen carbonate, and an aqueous solution saturated with NaCl solution in this order, and dried over magnesium sulfate. The solvent was removed by evaporation to obtain 29.19 g of diethyl N-(2-hydroxyimino- 4-methylpentanoyl)aminomalonate (Compound B-25) as a colorless oily substance.

後処理

  1. filtrationfiltered
  2. customThe filtrate was subjected to removal of the solvent by evaporation
  3. additionThe residue was mixed with ethyl acetate
  4. washthe mixture was washed with 10% hydrochloric acid, water
  5. dry with materialan aqueous solution saturated with sodium hydrogen carbonate, and an aqueous solution saturated with NaCl solution in this order, and dried over magnesium sulfate
  6. customThe solvent was removed by evaporation

出典と根拠

ORDレコード
ord-ef31f401088a47ffb34818fdf6261a76
出典データセット
uspto-grants-1993_08
特許番号
US05238938

反応ノート

読み込み中…