Potassium Carbonate → HCID 57597564, 화합물

HRID 1786555노트

반응식

HRID 1786555 반응식
Br[CH:2]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH2:15]([O:17][C:18]([C@@H:20]1[CH2:24][C@H:23]([NH:25][C:26](=[O:41])[CH2:27][CH:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH2:22][NH:21]1)=[O:19])[CH3:16].C([O-])([O-])=O.[K+].[K+]>CC(=O)CC>[CH2:15]([O:17][C:18]([C@@H:20]1[CH2:24][C@H:23]([NH:25][C:26](=[O:41])[CH2:27][CH:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH2:22][N:21]1[CH:2]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:19])[CH3:16]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 236603BromodiphenylmethaneHCID 57597565HCID 57597565, 화합물

생성물 1

HCID 57597564HCID 57597564, 화합물수율 57.2%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

To a solution of bromodiphenylmethane (0.4 g, 1.64 mmol) in butanone (10 ml) was added (2S,4S)-4-(3,3-diphenyl-propionylamino)-pyrrolidine-2-carboxylic acid ethyl ester (36) (0.6 g, 1.64 mmol), K2CO3 (0.23 g, 1.64 mmol) and KI (0.27 g, 1.64 mmol). The mixture was heated under reflux for 18 hours, and then filtered and the solvent was removed in vacuo. The residue was dissolved in CH2Cl2 (50 ml) and washed with water (10 ml). Drying over MgSO4 and removal of solvent under reduced pressure followed by column chromatography using Hex:EtOAc (1:1) gives 0.5 g the desired product.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 18 hours
  3. filtrationfiltered
  4. customthe solvent was removed in vacuo
  5. dissolutionThe residue was dissolved in CH2Cl2 (50 ml)
  6. washwashed with water (10 ml)
  7. dry with materialDrying over MgSO4 and removal of solvent under reduced pressure

출처 및 근거

ORD 기록
ord-bac9ddbcb8d04a9bba676089661f1a08
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07507760B2

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