Pyridine → HCID 20431430, 화합물

HRID 1263067

반응식

HRID 1263067 반응식
[C:1]([NH:6][CH2:7][C:8]([OH:10])=O)(=[O:5])[C:2]([CH3:4])=[CH2:3].Cl.[NH2:12][C:13]1[C:18]([OH:19])=[C:17]([Cl:20])[C:16]([CH3:21])=[C:15]([Cl:22])[CH:14]=1.N1C=CC=CC=1.S(Cl)(Cl)=O>O.C(OCC)(=O)C>[C:1]([NH:6][CH2:7][C:8]([NH:12][C:13]1[C:18]([OH:19])=[C:17]([Cl:20])[C:16]([CH3:21])=[C:15]([Cl:22])[CH:14]=1)=[O:10])(=[O:5])[C:2]([CH3:4])=[CH2:3]

참가 물질

7

반응물 4

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 152645N-Methacryloyl glycineHCID 1702236-Amino-2,4-dichloro-m-cresol hydrochloride

생성물 1

HCID 20431430HCID 20431430, 화합물수율 54.9%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To mixture composed of 68 g (0.48 mol) of N-methacryloyl glycine obtained in the above described manner and 46 g (0.2 mol) of 6-amino-2,4-dichloro-3-methylphenol hydrochloride were added 114 ml (1.44 mol) of pyridine and 1 liter of ethyl acetate and stirred under cooling. To the solution was added dropwise 29 ml (0.4 mol) of thionyl chloride. After the completion of the reaction, 300 ml of water was added to the reaction solution and extracted with ethyl acetate. The ethyl acetate solution was concentrated and to the residue was added acetonitrile. The crystals thus deposited were collected and recrystallized from acetonitrile to obtain 34.8 g of Monomer Coupler (2).

후처리

  1. customobtained in the
  2. temperatureunder cooling
  3. additionwas added to the reaction solution
  4. extractionextracted with ethyl acetate
  5. concentrationThe ethyl acetate solution was concentrated and to the residue
  6. additionwas added acetonitrile
  7. customThe crystals thus deposited were collected
  8. customrecrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-e138b3a795bc487b9dda14d35b363ac0
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04455366

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