Sodium hydride → Quinazoline, 4-(2-(1,1'-biphenyl)-4-ylethoxy)-

HRID 35842

反応式

HRID 35842 の反応式
[H-].[Na+].[C:3]1([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][OH:11])=[CH:5][CH:4]=1.Cl[C:19]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[N:22]=[CH:21][N:20]=1>CN(C=O)C.O>[C:3]1([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:4]=[CH:5][C:6]([CH2:9][CH2:10][O:11][C:19]2[C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[N:22]=[CH:21][N:20]=2)=[CH:7][CH:8]=1

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 788644-ChloroquinazolineHCID 64245772-[1,1'-Biphenyl]-4-yl-1-ethanol

生成物 1

HCID 180255Quinazoline, 4-(2-(1,1'-biphenyl)-4-ylethoxy)-収率 30.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of 0.53 g of sodium hydride in 200 ml of DMF was added 2.2 g of 2-[(1,1'-biphenyl)-4-yl]ethanol, and the mixture was stirred at room temperature for one hour. Then 1.8 g of 4-chloroquinazoline in 20 ml of DMF were added, and the mixture was stirred at room temperature for another three hours. The mixture was then poured into a mixture of ice in water. The solid phase was collected and washed with water. TLC showed two spots. The product was purified using HPLC (silica gel, CH2Cl2) giving 1.1 g of the title product. Yield: 30.6%. M.P. 72°-74° C.

後処理

  1. stirringthe mixture was stirred at room temperature for another three hours
  2. customThe solid phase was collected
  3. washwashed with water
  4. customThe product was purified

出典と根拠

ORDレコード
ord-7bb7da0e0d064691b38524fa0f9a41fd
出典データセット
uspto-grants-1995_05
特許番号
US05411963

関連ノート

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