Pyridine → HCID 20455716、化合物

HRID 1263065

反応式

HRID 1263065 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 20455716HCID 20455716、化合物収率 92.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5acdb209e07c4f12aa06d379c57af99f
出典データセット
uspto-grants-1984_06
特許番号
US04455366

関連ノート

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