Epichlorohydrin → 6-Chloro-7-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril

HRID 621552노트

반응식

HRID 621552 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[OH:12])[NH:8][C:7](=[O:13])[CH2:6][CH2:5]2.[OH-].[Na+].[CH2:16]([CH:18]1[O:20][CH2:19]1)Cl>CO>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH2:16][CH:18]1[O:20][CH2:19]1)[NH:8][C:7](=[O:13])[CH2:6][CH2:5]2

참가 물질

5

반응물 3

HCID 7835EpichlorohydrinHCID 14798Sodium Hydroxide2회HCID 128994206-Chloro-7-hydroxy-3,4-dihydrocarbostyril

생성물 1

HCID 128994376-Chloro-7-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

20.0 grams of 6-chloro-7-hydroxy-3,4-dihydrocarbostyril and 3.7 g of sodium hydroxide are mixed with 100 ml of methanol and stirred for 3 hours, then 150 ml of epichlorohydrin is added thereto and heated for 5 hours under refluxing conditions. After the reaction is completed, the reaction mixture is concentrated under reduced pressure to dryness. The residue thus obtained is mixed with 100 ml of 2N-sodium hydroxide and stirred well. The insoluble matter is separated by filtration, washed with water and dried. The crude crystals thus obtained are recrystallized from methanol-ethanol to obtain 19.7 g of 6-chloro-7-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril in the form of colorless crystals with a melting point of 190°-192° C.

후처리

  1. temperatureheated for 5 hours under refluxing conditions
  2. concentrationthe reaction mixture is concentrated under reduced pressure to dryness
  3. customThe residue thus obtained
  4. stirringstirred well
  5. customThe insoluble matter is separated by filtration
  6. washwashed with water
  7. customdried
  8. customThe crude crystals thus obtained
  9. customare recrystallized from methanol-ethanol

출처 및 근거

ORD 기록
ord-d807fc37cef644d8b02f38085e388b01
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824840

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