2-(Dimethylamino)ethanol → HCID 57889332、化合物

HRID 1016196ノート

反応式

HRID 1016196 の反応式
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]

参加物

8

反応物 5

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

生成物 1

HCID 57889332HCID 57889332、化合物

試薬・触媒・溶媒 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-23d9d80d2ed8492584bc3739cb0f7aad
出典データセット
uspto-grants-2011_07
特許番号
US07985861B2

反応ノート

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