Acetic Anhydride → 5-Acetyl-2,2'-bithienyl

HRID 1289116

반응식

HRID 1289116 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[S:7][CH:8]=[CH:9][CH:10]=1.[C:11](OC(=O)C)(=[O:13])[CH3:12]>P(=O)(O)(O)O>[C:11]([C:5]1[S:1][C:2]([C:6]2[S:7][CH:8]=[CH:9][CH:10]=2)=[CH:3][CH:4]=1)(=[O:13])[CH3:12]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 681202,2'-Bithiophene

생성물 1

HCID 6064225-Acetyl-2,2'-bithienyl

시약·촉매·용매 1

HCID 1004Phosphoric Acid촉매

실험 절차

2.40 g of 2,2'-bithiophene was dissolved in 8 ml of acetic anhydride and refluxed under nitrogen gas atmosphere. 6 drops of phosphoric acid (85%) was added and reacted for 5 hours. The reaction mixture was poured onto 200 g of crushed ice cubes and stirred for 1 h. The solid deposited was collected and vacuum distilled, 5-acetyl-2,2'-bithiophene 1.98 g was obtained at 148° C./0.8 mm-Hg and the melting point was 112°-113° C. The residue was recrystallized from dioxane and 0.25 g of 5,5'-diacetyl-2,2'-bithiophene with melting point of 236°-9° C. was obtained.

후처리

  1. temperaturerefluxed under nitrogen gas atmosphere
  2. customreacted for 5 hours
  3. customThe solid deposited was collected
  4. distillationvacuum distilled

출처 및 근거

ORD 기록
ord-f199d1ef7a284316bca550543d1654fe
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05747525

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