Hydrochloric Acid → N-(1.4-Dihydro-6.7-dichloro-2.3-dioxoquinoxaline-5-yl)-N-(3-pyridylmethyl)methanesulphonamide hydrochloride

HRID 1458556ノート

反応式

HRID 1458556 の反応式
[Cl:1][C:2]1[C:3]([N:17]([CH2:22][C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[S:18]([CH3:21])(=[O:20])=[O:19])=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[N:8]=[C:7]([O:13]C)[C:6]([O:15]C)=[N:5]2.Cl>O1CCOCC1>[ClH:1].[Cl:1][C:2]1[C:3]([N:17]([CH2:22][C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[S:18]([CH3:21])(=[O:20])=[O:19])=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[C:6](=[O:15])[NH:5]2

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 22097013N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(3-pyridylmethyl)methanesulphonamide

生成物 1

HCID 22097005N-(1.4-Dihydro-6.7-dichloro-2.3-dioxoquinoxaline-5-yl)-N-(3-pyridylmethyl)methanesulphonamide hydrochloride収率 181.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(3-pyridylmethyl)-methanesulphonamide (130 mg, 0.293 mmol), 2M hydrochloric acid (2 ml) and dioxane (4 ml) was heated at reflux for 2.5 hours, cooled, and concentrated under reduced pressure. The residue was suspended in water (1 ml), filtered off, and washed with water and ether to give the title compound (120 mg, 98%) as a white solid, m.p. 234°-235° C. (dec.).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 2.5 hours
  3. temperaturecooled
  4. concentrationconcentrated under reduced pressure
  5. filtrationfiltered off
  6. washwashed with water and ether

出典と根拠

ORDレコード
ord-115a64dcec294303b602f2f6f711fc17
出典データセット
uspto-grants-1998_12
特許番号
US05852016

反応ノート

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