2-(Dimethylamino)ethanol → HCID 57889332, 화합물

HRID 1820266노트

반응식

HRID 1820266 반응식
I[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.[NH2:8][C@@H:9]([C:13]([OH:15])=[O:14])[CH:10]([CH3:12])[CH3:11].CN(CCO)C.[O-]P([O-])([O-])=O.[K+].[K+].[K+].CO.O.C(O)(C(F)(F)F)=O>[Cu]I.O>[CH3:11][CH:10]([CH3:12])[C@@H:9]([NH:8][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1)[C:13]([OH:15])=[O:14]

참가 물질

8

반응물 5

HCID 79022-(Dimethylamino)ethanolHCID 62657Potassium Phosphate, TribasicHCID 707143-IodopyridineHCID 71563D-ValineHCID 21999908MeOH water TFA

생성물 1

HCID 57889332HCID 57889332, 화합물

시약·촉매·용매 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 962Water용매

실험 절차

3-Iodopyridine (525 mg, 2.58 mmol), D-valine (250 mg, 2.13 mmol), copper(I) iodide (40.6 mg, 0.213 mmol), dimethylaminoethanol (400 mg, 4.49 mmol), potassium phosphate tribasic (1359 mg, 6.40 mmol), and water (2 mL) was stirred at 80° C. overnight. The reaction was washed with EtOAc, then the aqueous portion was concentrated. The residue was slurried with MeOH and the MeOH portion was concentrated. The product was isolated using preparative reverse phase HPLC (MeOH/water/TFA) and used in next step without further purification.

후처리

  1. washThe reaction was washed with EtOAc
  2. concentrationthe aqueous portion was concentrated
  3. concentrationthe MeOH portion was concentrated
  4. customThe product was isolated
  5. customused in next step without further purification

출처 및 근거

ORD 기록
ord-be3d5c2615ad41c6a2f2b97e860dbf7c
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07601844B2

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