Benzenamine, 3-chloro-, hydrochloride (1:1) → Chloride

HRID 1068939

반응식

HRID 1068939 반응식
[C:1]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17]2[C:21]([C:22]#[N:23])=[C:20]([N:24](C)[CH3:25])[N:19](N=C)[N:18]=2)=[CH:12][CH:11]=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].Cl.[Cl:30][C:31]1[CH:32]=[C:33]([CH:35]=[CH:36][CH:37]=1)[NH2:34]>C(O)C>[Cl-:30].[C:1]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17]2[C:21]3[C:20](=[N:24][CH:25]=[N:23][C:22]=3[NH:34][C:33]3[CH:35]=[CH:36][CH:37]=[C:31]([Cl:30])[CH:32]=3)[NH:19][N:18]=2)=[CH:12][CH:11]=1)([O:3][C:4]([CH3:6])([CH3:7])[CH3:5])=[O:2]

참가 물질

5

반응물 2

HCID 67336Benzenamine, 3-chloro-, hydrochloride (1:1)HCID 696969723-[4-(N-Boc-aminomethyl)-phenylamino]-4-cyano-5-dimethylamino-methyleneamino-pyrazole

생성물 2

HCID 312ChlorideHCID 178453074HCID 178453074, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 94 g (245.1 mmol) of 3-[4-(N-Boc-aminomethyl)-phenylamino]-4-cyano-5-dimethylamino-methyleneamino-pyrazole, 44.2 g (269.4 mmol) of 3-chloro-aniline hydrochloride [for preparation see: Justus Liebigs Ann. Chem. 176, 45 (1875)] and 1000 ml of ethanol is heated under reflux for 60 hours and then concentrated by evaporation in vacuo. The residue is dissolved in ethyl acetate, and the organic phase is washed with ice-cold 0.5N hydrochloric acid, water and brine, dried over sodium sulfate and concentrated by evaporation in vacuo. After recrystallization of the residue from ethyl acetate/hexane and from methanolimethylene chloride, 3-[4-(N-Boc-aminomethyl)-phenylamino]-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine is obtained; m.p. 196° C.; ESI-MS: (M−H)−=464.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 60 hours
  3. concentrationconcentrated by evaporation in vacuo
  4. dissolutionThe residue is dissolved in ethyl acetate
  5. washthe organic phase is washed with ice-cold 0.5N hydrochloric acid, water and brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated by evaporation in vacuo
  8. customAfter recrystallization of the residue from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-dc2811f085cf4f53acfd123559381d8f
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06251911B1

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