Acrylic Acid → 3-(4-Bromo-3-methylphenylthio)propionic acid

HRID 129436

반응식

HRID 129436 반응식
[C:1]1([CH3:8])[CH:6]=[CH:5][CH:4]=[C:3]([SH:7])[CH:2]=1.[C:9]([OH:13])(=[O:12])[CH:10]=[CH2:11].[Br:14]Br.S([O-])(O)=O.[Na+]>C(O)(=O)C.C(N(CC)CC)C>[Br:14][C:6]1[CH:5]=[CH:4][C:3]([S:7][CH2:11][CH2:10][C:9]([OH:13])=[O:12])=[CH:2][C:1]=1[CH3:8]

참가 물질

7

반응물 4

HCID 6581Acrylic AcidHCID 79303-ThiocresolHCID 24408BromineHCID 23665763Sodium Bisulfite

생성물 1

HCID 233633233-(4-Bromo-3-methylphenylthio)propionic acid

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 8471Triethylamine용매

반응 조건

온도
50 °C

실험 절차

A one-liter, three-necked flask was charged with 0 g (0.4 mol) of m-toluenethiol, 29 g (0.4 mol) of acrylic acid and 1.0 ml of triethylamine and the mixture was allowed to react at 150° C. for 1 hour. After the reaction mixture was allowed to cool, 200 ml of acetic acid was added to the reaction mixture, and the mixture was heated up to 50° C. to form a complete solution. Then, 21 ml of bromine was gradually added over 30 minutes, and the mixture was further allowed to react at 50° to 50° C. for 1 hour. After the reaction was completed, the reaction mixture was poured into 1.5 liters of a 1% sodium hydrogensulfite aqueous solution, and the formed solid was recovered by filtration and dried to give 110 g of 3-(4-bromo-3-methylphenylthio)propionic acid as a crude product.

후처리

  1. customto react at 150° C. for 1 hour
  2. temperatureto cool
  3. customto form a complete solution
  4. customto react at 50° to 50° C. for 1 hour
  5. filtrationthe formed solid was recovered by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-650ed786722544959787f1db033e12b5
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05468722

연결된 노트

불러오는 중…