HCID 178418573、化合物 → HCID 178441847、化合物

HRID 486020ノート

反応式

HRID 486020 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-quinazoline-carboxaldehyde 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. CI MASS SPEC 247(MH+).

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-d3272f09e4f142268cd991445491ddc8
出典データセット
uspto-grants-1994_03
特許番号
US05290780

反応ノート

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