Dimethylformamide diethylacetal → HCID 178492224、化合物

HRID 1602256ノート

反応式

HRID 1602256 の反応式
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([NH:7][C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)[C:3]=1[C:16]#[N:17].C(O[CH:21](OCC)[N:22]([CH3:24])[CH3:23])C>C1(C)C=CC=CC=1>[C:16]([C:3]1[C:4]([NH:7][C:8]2[CH:9]=[CH:10][C:11]([O:14][CH3:15])=[CH:12][CH:13]=2)=[N:5][NH:6][C:2]=1[N:1]=[CH:21][N:22]([CH3:24])[CH3:23])#[N:17]

参加物

4

反応物 2

HCID 70913Dimethylformamide diethylacetalHCID 4646667112606-39-0

生成物 1

HCID 178492224HCID 178492224、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A suspension of 5.41 g (23.6 mmol) of 5-amino-4-cyano-3-(4-methoxy-phenylamino)-pyrazole [for preparation see: J. Heterocyclic Chem. 27, 775 (1990)] in 4.8 ml (27.2 mmol) of N,N-dimethylformamide diethyl acetal (97%) and 100 ml of toluene is heated under reflux for 5 hours. The reaction mixture is then cooled to room temperature and filtered and the filter residue is washed with toluene. Recrystallization of the crude product from methanol/water yields the title compound; m.p. 232-234° C. (decomp.).

後処理

  1. temperatureis heated
  2. temperatureunder reflux for 5 hours
  3. filtrationfiltered
  4. washthe filter residue is washed with toluene
  5. customRecrystallization of the crude product from methanol/water

出典と根拠

ORDレコード
ord-7ae223ca55de49c69f66c4cdcefda9db
出典データセット
uspto-grants-1999_11
特許番号
US05981533

反応ノート

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