Triethyl orthoacetate → HCID 178467957、化合物

HRID 46561

反応式

HRID 46561 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][C:12]=1[F:13])[C:5]([CH2:7][C:8]#[N:9])=[O:6].[C:14](OCC)(OCC)([O:16]CC)[CH3:15].CC(OCC1C2C(=CC=CC=2)C(COC(C)=O)=C2C=1C=CC=C2)=O>O>[F:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][C:12]=1[F:13])[C:5](/[C:7](=[C:14](/[OH:16])\[CH3:15])/[C:8]#[N:9])=[O:6]

参加物

5

反応物 3

HCID 66221Triethyl orthoacetateHCID 613145Acetic acid 10-acetoxymethyl-anthracen-9-ylmethyl esterHCID 27582543,4-Difluorobenzoylacetonitrile

生成物 1

HCID 178467957HCID 178467957、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 10.2 g. of 3,4-difluorobenzoylacetonitrile, 9.2 g. of triethyl orthoacetate and 20 ml. of acetic anhyride is heated on a steam bath for 0.5 hour and then poured into 200 ml. of water which is then heated on the steam bath for 2 hours. On cooling, the solid is filtered and then dissolved in methylene chloride. This solution is extracted with two portions of aqueous sodium bicarbonate and the aqueous extracts are combined and acidified with concentrated hydrochloric acid. The precipitate is extracted into methylene chloride, passed through a pad of Magnesol®, heated and diluted with hexane. Upon cooling, colorless crystals result, yielding the title compound, m.p. 51°-54° C.

後処理

  1. additionpoured into 200 ml
  2. temperatureOn cooling
  3. filtrationthe solid is filtered
  4. dissolutiondissolved in methylene chloride
  5. extractionThis solution is extracted with two portions of aqueous sodium bicarbonate
  6. extractionThe precipitate is extracted into methylene chloride
  7. temperatureheated
  8. additiondiluted with hexane
  9. temperatureUpon cooling
  10. customcolorless crystals result

出典と根拠

ORDレコード
ord-9758583a2e034c5e851606c75fa8cd98
出典データセット
uspto-grants-1979_11
特許番号
US04173650

関連ノート

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