7-[3-(Trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrile → HCID 135773307、化合物

HRID 231510

反応式

HRID 231510 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.C([BH3-])#N.[Na+]>C(O)(=O)C>[F:20][C:2]([F:1])([F:21])[C:3]1[CH:4]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]#[N:19])=[C:13]3[NH:12][CH2:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 27410147-[3-(Trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrileHCID 5003444Sodium cyanoborohydride

生成物 1

HCID 135773307HCID 135773307、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 6.0 g of 7-(α,α,α-trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine-3-carbonitrile (Ex. 3, U.S. Pat. No. 4,236,005) in 100 ml of glacial acetic acid, was added in portions, 3.0 g of sodium cyanoborohydride at room temperature under nitrogen. The mixture was stirred at room temperature for 2 hours. The precipitate was collected by filtration, washed with water, then dissolved in dichloromethane. The organic solution was neutralized with a saturated solution of sodium bicarbonate, then dried over anhydrous sodium sulfate and filtered. The filtrate was evaporated in vacuo and gave the desired product as a white solid. The product was recrystallized from isopropyl alcohol, mp 175°-177° C.

後処理

  1. filtrationThe precipitate was collected by filtration
  2. washwashed with water
  3. dissolutiondissolved in dichloromethane
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customThe filtrate was evaporated in vacuo

出典と根拠

ORDレコード
ord-8031aa026700490d9a59d611704f7ea8
出典データセット
uspto-grants-1989_07
特許番号
US04847256

関連ノート

読み込み中…