HCID 178418573、化合物 → HCID 178441847、化合物

HRID 487054ノート

反応式

HRID 487054 の反応式
[CH2:1]([C:5]1[NH:6][C:7]2[C:12]([C:13](=[O:15])[N:14]=1)=[CH:11][C:10]([CH:16]=[O:17])=[CH:9][CH:8]=2)[CH2:2][CH2:3][CH3:4].[CH3:18][Mg]Br>O1CCCC1.C(OCC)C>[CH2:1]([C:5]1[NH:6][C:7]2[C:12]([C:13](=[O:15])[N:14]=1)=[CH:11][C:10]([CH:16]([OH:17])[CH3:18])=[CH:9][CH:8]=2)[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 2

HCID 178418573HCID 178418573、化合物HCID 178441857HCID 178441857、化合物

生成物 1

HCID 178441847HCID 178441847、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a solution of 0.60 g of 2-butyl-1,4-dihydro-4-oxo-6-quinazolinecarboxaldehyde in 30 ml of dry tetrahydrofuran, cooled to 0° C. is added dropwise, 2.61 ml of a 3.0M solution of methylmagnesium bromide in diethyl ether. The reaction is stirred at 0° C. for 30 minutes and then quenched with 10 ml of aqueous ammonium chloride. After diluting with 10 ml of water, the reaction mixture is extracted with 9:1 chloroform-methanol. The combined extracts are dried with magnesium sulfate, filtered and concentrated to yield 0.64 g of the desired product.

後処理

  1. additionis added dropwise
  2. customquenched with 10 ml of aqueous ammonium chloride
  3. additionAfter diluting with 10 ml of water
  4. extractionthe reaction mixture is extracted with 9:1 chloroform-methanol
  5. dry with materialThe combined extracts are dried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-d2da8b328fa14a7c94cc7d2fd6e558d3
出典データセット
uspto-grants-1994_03
特許番号
US05294611

反応ノート

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