Dicyclohexylcarbodiimide → HCID 86747153, 화합물

HRID 2255163노트

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HRID 2255163 반응식
[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]

참가 물질

6

반응물 4

HCID 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 81272Propanedioic acid, 2-amino-, 1,3-diethyl ester2회HCID 92779(+-)-2-Hydroxyisocaproic acid

생성물 1

HCID 86747153HCID 86747153, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ef31f401088a47ffb34818fdf6261a76
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05238938

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