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

HRID 1075734노트

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HRID 1075734 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

반응 조건

온도
30 °C

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-fa0af7695faf46469d91ee55cf86e874
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03954442

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