4-Methylmorpholine → N-[N2-[(1,1-dimethylethoxy) carbonyl]-N6-[(phenylmethoxy)carbonyl]-L-lysinyl]-L-alanine 1,1-dimethylethyl ester

HRID 34492

반응식

HRID 34492 반응식
CN1CCOCC1.[CH3:8][C:9]([O:12][C:13](=[O:17])[C@H:14]([CH3:16])[NH2:15])([CH3:11])[CH3:10].N#N.[CH3:20][C:21]([CH3:46])([O:23][C:24]([NH:26][C@H:27]([C:43](O)=[O:44])[CH2:28][CH2:29][CH2:30][CH2:31][NH:32][C:33]([O:35][CH2:36][C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)=[O:34])=[O:25])[CH3:22].Cl.CN(C)CCCN=C=NCC.ON1C2C=CC=CC=2N=N1>ClCCl>[CH3:8][C:9]([O:12][C:13](=[O:17])[C@H:14]([CH3:16])[NH:15][C:43](=[O:44])[C@H:27]([CH2:28][CH2:29][CH2:30][CH2:31][NH:32][C:33]([O:35][CH2:36][C:37]1[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=1)=[O:34])[NH:26][C:24]([O:23][C:21]([CH3:46])([CH3:20])[CH3:22])=[O:25])([CH3:11])[CH3:10]

참가 물질

7

반응물 5

HCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 89016L-Alanine 1,1-dimethylethyl esterHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 86742311N2 [(1,1-dimethylethoxy)carbonyl]-N6-[(phenylmethoxy)carbonyl]-L-lysine

생성물 1

HCID 53963310N-[N2-[(1,1-dimethylethoxy) carbonyl]-N6-[(phenylmethoxy)carbonyl]-L-lysinyl]-L-alanine 1,1-dimethylethyl ester수율 90.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

N-Methylmorpholine (3.3 ml) was added to a suspension of L-alanine 1,1 -dimethylethyl ester (4.0 g), N2 -[(1,1-dimethylethoxy)carbonyl]-N6 -[(phenylmethoxy)carbonyl]-L-lysine (11.4 g), N-(3-dimethylaminopropyl)-N'-ethylcarbodiimide hydrochloride (5.8 g) and 1-hydroxybenzotriazole (4.1 g) in dichloromethane (150 ml). The resulting mixture was allowed to stand for 18 hours, and was then poured into distilled water (200 ml). The organic phase was separated, washed with water, saturated sodium hydrogen carbonate, dilute aqueous citric acid, brine and dried over anhydrous magnesium sulphate. The solvent was removed under reduced pressure to yield N-[N2 -[(1,1-dimethylethoxy) carbonyl]-N6 -[(phenylmethoxy)carbonyl]-L-lysinyl]-L-alanine 1,1-dimethylethyl ester (12.6 g) as a foam.

후처리

  1. additionwas then poured
  2. distillationinto distilled water (200 ml)
  3. customThe organic phase was separated
  4. washwashed with water, saturated sodium hydrogen carbonate, dilute aqueous citric acid, brine
  5. dry with materialdried over anhydrous magnesium sulphate
  6. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-24498aec61e446009080dc62880529ac
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04761483

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