1,2-Dichloroethane → HCID 16617197, 화합물

HRID 456426

반응식

HRID 456426 반응식
[C:1]1([CH:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:8][C:9]([OH:11])=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:18]([N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1)([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19].C(Cl)CCl>C(Cl)Cl.CN(C1C=CN=CC=1)C>[C:21]([O:20][C:18]([N:25]1[CH2:30][CH2:29][N:28]([C:9](=[O:11])[CH2:8][CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:27][CH2:26]1)=[O:19])([CH3:24])([CH3:22])[CH3:23]

참가 물질

6

반응물 3

HCID 111,2-DichloroethaneHCID 64798Diphenylpropionic acidHCID 143452tert-Butyl piperazine-1-carboxylate

생성물 1

HCID 16617197HCID 16617197, 화합물수율 76%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

To a solution of 3,3 diphenylpropionic acid (1.45 g, 6.44 mmol) in dry CH2Cl2 (70 ml) was added mono-boc piperizine (1.32 g, 7.08 mmol) under nitrogen. To the reaction was added EDC (2.71 g, 14.16 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) (200 ml). The organic was washed with water (50 ml, 2×) and 10% NaOH (50 ml) and dried over MgSO4 and evaporated to dryness. The resulting residue was purified by column chromatography using hexane:ethyl acetate (1:1) to give desired product in 76% yield.

후처리

  1. concentrationThe reaction was then concentrated under reduced pressure
  2. dissolutionThe residue dissolved in ethyl acetate:water (10:1) (200 ml)
  3. washThe organic was washed with water (50 ml, 2×) and 10% NaOH (50 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-ee02d08eb79742d4a63b30f30e66855e
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07186726B2

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