1-Bromo-3-chloropropane → N-[3-(3-Chloropropoxy)phenyl]urea

HRID 1709835

반응식

HRID 1709835 반응식
[OH:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]([NH2:11])=[O:10])[CH:5]=[CH:6][CH:7]=1.Br[CH2:13][CH2:14][CH2:15][Cl:16].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:16][CH2:15][CH2:14][CH2:13][O:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]([NH2:11])=[O:10])[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 12796m-Hydroxyphenylurea

생성물 1

HCID 14407185N-[3-(3-Chloropropoxy)phenyl]urea수율 83.1%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 45.6 g (0.3 mole of 1-(3-hydroxyphenyl)urea, 94.5 g (0.6 mole) of 1-bromo-3-chloropropane, 124.4 g (0.9 mole) of anhydrous potassium carbonate and 1 liter of acetone was heated at reflux with mechanical stirring for 20 hr. The mixture was concentrated and the residue was slurried with 1.5 liters of water. The mixture was filtered and the filter cake was recrystallized from 2-propanol to yield 57.0 g (83%) of off-white solid, m.p. 141°-143° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux
  3. concentrationThe mixture was concentrated
  4. filtrationThe mixture was filtered
  5. customthe filter cake was recrystallized from 2-propanol

출처 및 근거

ORD 기록
ord-1630cbfc37ce4f36940b1fad5cd4f519
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04950674

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