4-Methylmorpholine → HCID 66660968, 화합물

HRID 910406

반응식

HRID 910406 반응식
Cl.[CH3:2][O:3][C:4](=[O:10])[C@@H:5]([CH:7]([CH3:9])[CH3:8])[NH2:6].C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.[C:32]([NH:39][C@H:40]([C:49](O)=[O:50])[CH2:41][CH2:42][C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33].CN1CCOCC1>CN(C=O)C>[CH3:2][O:3][C:4](=[O:10])[CH:5]([NH:6][C:49](=[O:50])[CH:40]([NH:39][C:32]([O:34][C:35]([CH3:37])([CH3:36])[CH3:38])=[O:33])[CH2:41][CH2:42][C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)[CH:7]([CH3:9])[CH3:8]

참가 물질

7

반응물 5

HCID 79724-MethylmorpholineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 7018726(2S)-2-(((tert-butoxy)carbonyl)amino)-4-phenylbutanoic acidHCID 11984198Methyl D-valinate hydrochloride

생성물 1

HCID 66660968HCID 66660968, 화합물수율 142.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To an ice-cooled solution of D-valine methyl ester hydrochloride (1000 mg, 3.58 mmol) and HOBt (in DMF (14 mL) was added EDCI (755 mg, 3.94 mmol). After the mixture was stirred for 30 min, N-boc-L-homophenylalanine (600 mg, 3.58 mmol) and N-methylmorpholine (1 mL, 8.95 mmol) were added. The mixture was warmed to room temperature and stirred overnight. The solvent was removed and the residue was partitioned between water and EtOAc. The aqueous layer was extracted with EtOAc and the combined organic phases were dried over anhydrous Na2SO4. After concentration under reduced pressure, the crude title compound (2000 mg) was obtained and used in the next step without further purification.

후처리

  1. stirringstirred overnight
  2. customThe solvent was removed
  3. customthe residue was partitioned between water and EtOAc
  4. extractionThe aqueous layer was extracted with EtOAc
  5. dry with materialthe combined organic phases were dried over anhydrous Na2SO4
  6. concentrationAfter concentration under reduced pressure

출처 및 근거

ORD 기록
ord-5fb008c1333246cdb0cbc165b6a859a0
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022092B2

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