Ammonia → 3-Fluoro-4-(5-pentyl-1,3-dioxan-2-yl)-benzonitrile

HRID 246875

反応式

HRID 246875 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH:11]1[O:16][CH2:15][CH:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:13][O:12]1)[C:5](O)=O.O=S(Cl)Cl.[NH3:26]>>[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH:11]1[O:16][CH2:15][CH:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:13][O:12]1)[C:5]#[N:26]

参加物

4

反応物 3

HCID 222AmmoniaHCID 24386Thionyl ChlorideHCID 201624993-Fluoro-4-(5-pentyl-1,3-dioxan-2-yl)-benzoic acid

生成物 1

HCID 201621573-Fluoro-4-(5-pentyl-1,3-dioxan-2-yl)-benzonitrile

反応条件

温度
20 °C

実験手順

As described in Example 9 4.44 gms. of 3-fluoro-4-(5-pentyl-1,3-dioxan-2-yl)-benzoic acid are converted by SOCl2 into the acid chloride. After removing excess SOCl2 the residue obtained is added to aqueous ammonia and stirred for 4 hours at 20° C. The precipitated acid amide is filtrated by suction and dried. For conversion into the nitrile it is dissolved in 50 ml of pyridine and 10 ml of POCl3, then stirred at 20° C. for 20 hours and evaporated. Thus 3-fluoro-4-(5-pentyl-1,3-dioxan-2-yl)-benzonitrile is obtained.

後処理

  1. customAfter removing excess SOCl2 the residue
  2. customobtained
  3. filtrationThe precipitated acid amide is filtrated by suction
  4. customdried
  5. dissolutionFor conversion into the nitrile it is dissolved in 50 ml of pyridine
  6. stirring10 ml of POCl3, then stirred at 20° C. for 20 hours
  7. customevaporated

出典と根拠

ORDレコード
ord-b642ce8d36d54bfcaaa5052a39948671
出典データセット
uspto-grants-1987_11
特許番号
US04704227

関連ノート

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