1,2-Dichloroethane → HCID 11445050, 화합물

HRID 1295865노트

반응식

HRID 1295865 반응식
[NH2:1][CH2:2][CH:3]1[CH2:7][CH2:6][N:5]([C:8](=[O:28])[CH2:9][CH2:10][CH2:11][CH2:12][CH:13]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)[C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)[CH2:4]1.[C:29]([C:33]1[CH:34]=[C:35]([CH:39]=[C:40]([C:44]([CH3:47])([CH3:46])[CH3:45])[C:41]=1[O:42][CH3:43])[C:36](O)=[O:37])([CH3:32])([CH3:31])[CH3:30].C(Cl)CCl>C(Cl)Cl.CN(C1C=CN=CC=1)C>[F:20][C:17]1[CH:18]=[CH:19][C:14]([CH:13]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)[CH2:12][CH2:11][CH2:10][CH2:9][C:8]([N:5]2[CH2:6][CH2:7][CH:3]([CH2:2][NH:1][C:36](=[O:37])[C:35]3[CH:39]=[C:40]([C:44]([CH3:45])([CH3:46])[CH3:47])[C:41]([O:42][CH3:43])=[C:33]([C:29]([CH3:32])([CH3:31])[CH3:30])[CH:34]=3)[CH2:4]2)=[O:28])=[CH:15][CH:16]=1

참가 물질

6

반응물 3

HCID 111,2-DichloroethaneHCID 22324252HCID 22324252, 화합물HCID 58911294HCID 58911294, 화합물

생성물 1

HCID 11445050HCID 11445050, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(3-aminomethyl-pyrrolidin-1-yl)-6,6-bis-(4-fluoro-phenyl)-hexan-1-one (0.49 g, 1.26 mmol) in dry CH2Cl2 (35 ml) was added 3,5-di-tert-butyl-4-methoxy benzoic acid (0.33 g, 1.26 mmol) under nitrogen. To the reaction was added EDC (0.48 g, 2.52 mmol) and DMAP (cat) and the reaction mixture stirred under nitrogen at room temperature overnight. The reaction was then concentrated under reduced pressure. The residue dissolved in ethyl acetate: water (10:1) (130 ml). The organic was washed with water (30 ml, 2×) and 10% NaOH (30 ml) and dried over MgSO4 and evaporated to dryness. The resulting residue was purified by column chromatography using CH2Cl2:CH3OH (15:1) to give a desired product in good yield.

후처리

  1. concentrationThe reaction was then concentrated under reduced pressure
  2. dissolutionThe residue dissolved in ethyl acetate: water (10:1) (130 ml)
  3. washThe organic was washed with water (30 ml, 2×) and 10% NaOH (30 ml)
  4. dry with materialdried over MgSO4
  5. customevaporated to dryness
  6. customThe resulting residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-02bb372733d44eb0905cb1127104593d
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244758B2

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