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

HRID 1957991노트

반응식

HRID 1957991 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-31c959b9d76542829d67c3f973ab4e2f
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410100B2

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