Iodine → 7-chloro-4,5-dihydro-3-(2-iodoethynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

HRID 1606992

反応式

HRID 1606992 の反応式
[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[N:9]([CH3:18])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]#[CH:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].[I:22]I>CO.O>[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[N:9]([CH3:18])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]#[C:17][I:22])[C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 807IodineHCID 14798Sodium HydroxideHCID 198515337-chloro-3-ethynyl-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

生成物 1

HCID 198515167-chloro-4,5-dihydro-3-(2-iodoethynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

2.72 g (10 mmol) of 7-chloro-3-ethynyl-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one was suspended in 30 ml of methanol and cooled to 10°. There were then added simultaneously thereto in portions within about 10 minutes 5 ml of 28% sodium hydroxide solution and 3 g of iodine. After stirring at room temperature for 1 hour the suspension was diluted with about 30 ml of water, suction filtered and the suction filter cake was dried. By two recrystallizations from methylene chloride and ethyl acetate and from dioxane there was obtained 7-chloro-4,5-dihydro-3-(2-iodoethynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 215°-216°.

後処理

  1. temperaturecooled to 10°
  2. additionThere were then added simultaneously
  3. filtrationfiltered
  4. filtrationthe suction filter cake
  5. customwas dried
  6. customBy two recrystallizations from methylene chloride and ethyl acetate

出典と根拠

ORDレコード
ord-7c5d21ccf5ea48d69ca4307184a1ac4d
出典データセット
uspto-grants-1989_09
特許番号
US04863920

関連ノート

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