Hydrochloric Acid → 8-isopropyl-5-methyl-2-(3-nitro-5-trifluoromethyl-phenylamino)-7,8-dihydro-5H-pteridin-6-one

HRID 1957991ノート

反応式

HRID 1957991 の反応式
Cl[C:2]1[N:11]=[CH:10][C:9]2[N:8]([CH3:12])[C:7](=[O:13])[CH2:6][N:5]([CH:14]([CH3:16])[CH3:15])[C:4]=2[N:3]=1.[N+:17]([C:20]1[CH:21]=[C:22]([NH2:30])[CH:23]=[C:24]([C:26]([F:29])([F:28])[F:27])[CH:25]=1)([O-:19])=[O:18].Cl>O.O1CCOCC1>[CH:14]([N:5]1[C:4]2[N:3]=[C:2]([NH:30][C:22]3[CH:23]=[C:24]([C:26]([F:29])([F:28])[F:27])[CH:25]=[C:20]([N+:17]([O-:19])=[O:18])[CH:21]=3)[N:11]=[CH:10][C:9]=2[N:8]([CH3:12])[C:7](=[O:13])[CH2:6]1)([CH3:16])[CH3:15]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 27757093-Nitro-5-(trifluoromethyl)anilineHCID 584059002-chloro-8-isopropyl-5-methyl-7,8-dihydro-5H-pteridin-6-one

生成物 1

HCID 684223458-isopropyl-5-methyl-2-(3-nitro-5-trifluoromethyl-phenylamino)-7,8-dihydro-5H-pteridin-6-one収率 49%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

2-Chloro-8-isopropyl-5-methyl-7,8-dihydro-5H-pteridin-6-one of (2 g; 8.30 mmol) and 3-nitro-5-trifluoromethyl-phenylamine (1.71 g; 8.30 mmol) were diluted in 10 ml of water and 10 ml of 1,4-dioxane. 2 ml of HCl 37% were added. The reaction mixture was refluxed 48 h, then cooled to room temperature. The desired product precipitated from the reaction mixture, so, it was filtered, washed with water and dried in vacuo. Recrystallisation with 1,4-dioxane/water 1:1 gave 1.65 g (4.04 mmol; 49% yield) of white-yellow powder.

後処理

  1. temperatureThe reaction mixture was refluxed 48 h
  2. customThe desired product precipitated from the reaction mixture
  3. filtrationso, it was filtered
  4. washwashed with water
  5. customdried in vacuo
  6. customRecrystallisation with 1,4-dioxane/water 1:1
  7. customgave 1.65 g (4.04 mmol; 49% yield) of white-yellow powder

出典と根拠

ORDレコード
ord-31c959b9d76542829d67c3f973ab4e2f
出典データセット
uspto-grants-2013_04
特許番号
US08410100B2

反応ノート

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