Potassium Phosphate, Tribasic → HCID 56940822、化合物

HRID 1844038ノート

反応式

HRID 1844038 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][CH2:7][NH:8][C:9]2=[O:12])=[CH:4][CH:3]=1.Br[C:14]1[CH:15]=[N:16][CH:17]=[CH:18][C:19]=1[CH2:20][CH3:21].P([O-])([O-])([O-])=O.[K+].[K+].[K+]>[Cu](I)I.O1CCOCC1>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][CH2:7][N:8]([C:14]3[CH:15]=[N:16][CH:17]=[CH:18][C:19]=3[CH2:20][CH3:21])[C:9]2=[O:12])=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 62657Potassium Phosphate, TribasicHCID 131605333-Bromo-4-ethylpyridineHCID 186723977-Chloro-3,4-dihydroisoquinolin-1(2H)-one

生成物 1

HCID 56940822HCID 56940822、化合物収率 15.8%

試薬・触媒・溶媒 2

HCID 83717Copper iodide触媒HCID 312751,4-Dioxane溶媒

実験手順

7-Chloro-3,4-dihydroisoquinolin-1(2H)-one (I-1d: 100 mg, 0.552 mmol) was reacted with 3-bromo-4-ethyl pyridine (133.5 mg, 0.718 mmol), 1,4-dioxane (5 mL), copper iodide (10.48 mg, 0.0555 mmol), trans-N,N′-dimethyl-cyclohexyl-1,2-diamine (7.8 mg, 0.055 mmol) and potassium phosphate (351 mg, 1.657 mmol for 48 hours at 120° C. to afford the crude product. Purification by column chromatography on silica gel (50% ethyl acetate in hexane), followed by preparative HPLC afforded 25 mg of the product (15.72% yield).

後処理

  1. customto afford the crude product
  2. customPurification by column chromatography on silica gel (50% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-a12a2fa902b94b3ca98dbf5647067d9a
出典データセット
uspto-grants-2015_02
特許番号
US08946260B2

反応ノート

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