Sulfuric Acid → 7-[3-(Trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carboxamide

HRID 231497

反応式

HRID 231497 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]#[N:19])=[C:13]3[N:12]=[CH:11][CH:10]=2)[CH:4]=1.S(=O)(=O)(O)[OH:23]>>[F:21][C:2]([F:20])([F:1])[C:3]1[CH:4]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:19])=[O:23])=[C:13]3[N:12]=[CH:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1

参加物

3

反応物 2

HCID 1118Sulfuric AcidHCID 27410147-[3-(Trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrile

生成物 1

HCID 27776927-[3-(Trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carboxamide

実験手順

A mixture of 3.0 g of 7-(α,α,α-trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine-3-carbonitrile (prepared as described in U.S. Pat. No. 4,236,005) and 150 ml of concentrated sulfuric acid was stirred at room temperature for 4 hours. The solution was then carefully poured into ice water with stirring. The white precipitate formed was collected, washed with water and then with saturated sodium bicarbonate until it was neutral. The solid was heated with one liter of isopropyl alcohol and filtered. The white solid was dried in vacuo and gave the product of the example as a colorless solid, mp 256°-258° C.

後処理

  1. customprepared
  2. customThe white precipitate formed
  3. customwas collected
  4. washwashed with water
  5. temperatureThe solid was heated with one liter of isopropyl alcohol
  6. filtrationfiltered
  7. customThe white solid was dried in vacuo
  8. customgave the product of the example as a colorless solid, mp 256°-258° C.

出典と根拠

ORDレコード
ord-d3472c065766477b9134492fd67c1753
出典データセット
uspto-grants-1989_07
特許番号
US04847256

関連ノート

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