Methylamine → 4-(4-Chlorophenoxy)-alpha-phenoxypropionic acid methyl amide

HRID 1075734ノート

反応式

HRID 1075734 の反応式
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:18]=[CH:17][C:10]([O:11][CH:12]([CH3:16])[C:13](Cl)=[O:14])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.ClC1C=CC(OC2C=CC(OC(C)C(O)=O)=CC=2)=CC=1.S(Cl)(Cl)=O.[CH3:45][NH2:46]>C1C=CC=CC=1>[CH3:45][NH:46][C:13](=[O:14])[CH:12]([O:11][C:10]1[CH:17]=[CH:18][C:7]([O:6][C:5]2[CH:19]=[CH:20][C:2]([Cl:1])=[CH:3][CH:4]=2)=[CH:8][CH:9]=1)[CH3:16]

参加物

6

反応物 4

HCID 6329MethylamineHCID 24386Thionyl ChlorideHCID 64928ClofopHCID 129528252-(4-(4-Chlorophenoxy)phenoxy)propionic acid chloride

生成物 1

HCID 129528264-(4-Chlorophenoxy)-alpha-phenoxypropionic acid methyl amide

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
30 °C

実験手順

32 Grams of 4-(4-chlorophenoxy)-α-phenoxy-propionic acid chloride, prepared from 4-(4-chlorophenoxy)-α-phenoxypropionic acid (Example 5) and thionyl chloride, were dissolved in 150 ml of benzene and 7 grams of methyl amine were introduced at 15°C into the solution obtained. To complete the reaction the solution was stirred for 1 hour at 30°C, the precipitate formed was filtered off with suction, the benzenic solution was washed with water, dried over Na2SO4 and concentrated. The isolated crystals were recrystallized from petroleum ether. 28 Grams of 4-(4-chlorophenoxy)-α-phenoxypropionic acid methyl amide melting at 117° - 118°C were obtained. ##SPC6##

後処理

  1. customobtained
  2. customthe reaction the solution
  3. customthe precipitate formed
  4. filtrationwas filtered off with suction
  5. washthe benzenic solution was washed with water
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated
  8. customThe isolated crystals were recrystallized from petroleum ether

出典と根拠

ORDレコード
ord-fa0af7695faf46469d91ee55cf86e874
出典データセット
uspto-grants-1976_05
特許番号
US03954442

反応ノート

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