Hydrochloric Acid → HCID 20494720、化合物

HRID 1075301ノート

反応式

HRID 1075301 の反応式
[H-].[Na+].[CH:3]([N:6]1[CH:15]2[CH:10]([CH2:11][CH2:12][C:13]([CH3:16])=[CH:14]2)[C:9](=O)[NH:8][C:7]1=[O:18])([CH3:5])[CH3:4].[F:19][C:20]1[CH:25]=[CH:24][C:23]([Mg]Br)=[CH:22][CH:21]=1.Cl>O1CCCC1>[CH:3]([N:6]1[CH:15]2[CH:10]([CH2:11][CH2:12][C:13]([CH3:16])=[CH:14]2)[C:9]([C:23]2[CH:24]=[CH:25][C:20]([F:19])=[CH:21][CH:22]=2)=[N:8][C:7]1=[O:18])([CH3:5])[CH3:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 20494718HCID 20494718、化合物HCID 178418676HCID 178418676、化合物

生成物 1

HCID 20494720HCID 20494720、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred suspension of 2.37 g sodium hydride in 45 ml tetrahydrofurane are added portionwise at room temperature 13.32 g 1-isopropyl-7-methyl-4a,5,6,8a-tetrahydro-2,4-(1H)-quinazolindione and the mixture stirred for 45 minutes. 39 ml of a 2N solution of 4-fluorophenyl magnesium bromide in tetrahydrufurane are then added dropwise within 2 hours at an internal temperature of 40° and the resulting suspension stirred at 40° for 15 hours. 23 ml 15% hydrochloric acid are then added under ice cooling and the solvent removed in vacuo. The residue is taken up with water and methylene chloride. The methylene chloride phase is evaporated to dryness to obtain the title compound.

後処理

  1. stirringthe resulting suspension stirred at 40° for 15 hours
  2. customthe solvent removed in vacuo
  3. customThe methylene chloride phase is evaporated to dryness

出典と根拠

ORDレコード
ord-eed2d5ed1314469eab0cda1878898ecf
出典データセット
uspto-grants-1983_07
特許番号
US04395550

反応ノート

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