Acetic Acid → 2,3,4-Tribromo-5-(chloromethyl)thiophene

HRID 460968

反応式

HRID 460968 の反応式
C=O.[ClH:3].[Br:4][C:5]1[C:9]([Br:10])=[C:8]([Br:11])[S:7][CH:6]=1.[C:12](O)(=O)C>>[Cl:3][CH2:12][C:6]1[S:7][C:8]([Br:11])=[C:9]([Br:10])[C:5]=1[Br:4]

参加物

5

反応物 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 712Formaldehyde2 回HCID 765932,3,4-Tribromothiophene

生成物 1

HCID 151249082,3,4-Tribromo-5-(chloromethyl)thiophene

反応条件

温度
70 °C

実験手順

4.07 G. (50 mmol) of formalin (37%) and 40 ml. of concentrated hydrochloric acid were added to a solution of 10.2 g. (33.3 mmol) of 3,4,5-tribromothiophene in 20 ml. of acetic acid. The resulting mixture was warmed to 70° C. After 6 hrs., 4.07 g. of formalin were added and heating was continued overnight. The resulting mixture was cooled, poured on ice water and extracted with ether. The organic phase was washed twice with water, sodium bicarbonate and water, dried and evaporated to give crude 2-chloromethyl-3,4,5-tribromothiophene.

後処理

  1. temperatureheating
  2. waitwas continued overnight
  3. temperatureThe resulting mixture was cooled
  4. additionpoured on ice water
  5. extractionextracted with ether
  6. washThe organic phase was washed twice with water, sodium bicarbonate and water
  7. customdried
  8. customevaporated

出典と根拠

ORDレコード
ord-408a0434d5404f2d8ed59b0a849175be
出典データセット
uspto-grants-1977_12
特許番号
US04061656

関連ノート

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