4-Methylmorpholine → HCID 66660968、化合物

HRID 910406

反応式

HRID 910406 の反応式
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]

参加物

7

反応物 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

生成物 1

HCID 66660968HCID 66660968、化合物収率 142.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5fb008c1333246cdb0cbc165b6a859a0
出典データセット
uspto-grants-2011_09
特許番号
US08022092B2

関連ノート

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