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

HRID 460968

반응식

HRID 460968 반응식
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]

참가 물질

5

반응물 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 712Formaldehyde2회HCID 765932,3,4-Tribromothiophene

생성물 1

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

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-408a0434d5404f2d8ed59b0a849175be
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04061656

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