Pyridine → HCID 20455716, 화합물

HRID 1263065

반응식

HRID 1263065 반응식
[Cl:1][CH:2]([CH3:10])[C:3]([NH:5][CH2:6][C:7]([OH:9])=O)=[O:4].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(#N)C>[Cl:1][CH:2]([CH3:10])[C:3]([NH:5][CH2:6][C:7]([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:9])=[O:4]

참가 물질

7

반응물 4

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 1702236-Amino-2,4-dichloro-m-cresol hydrochlorideHCID 20455717N-(2-Chloropropanoyl)glycine

생성물 1

HCID 20455716HCID 20455716, 화합물수율 92.2%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

To a mixture composed of 158 g (0.96 mol) of N-(β-chloropropanoyl)glycine thus obtained and 92 g (0.4 mol) of 6-amino-2,4-dichloro-3-methylphenol hydrochloride were added 228 ml (2.88 mol) of pyridine and 2 liters of acetonitrile and stirred under cooling. To the solution was added dropwise 95.2 g (0.8 mol) of thionyl chloride. After the completion of the reaction, water was added to the reaction solution and the crystals thus deposited were collected by filtration and recrystallized from acetonitrile to obtain 125.2 g of 6-[α-(β-chloropropanamido)acetamido]-2,4-dichloro-3-methylphenol.

후처리

  1. customthus obtained
  2. temperatureunder cooling
  3. additionwas added to the reaction solution
  4. filtrationthe crystals thus deposited were collected by filtration
  5. customrecrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-5acdb209e07c4f12aa06d379c57af99f
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04455366

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