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1-Bromo-3-chloropropane → HCID 12899443, 화합물

HRID 621553
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HRID 621553 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([Br:13])[C:11]=1[OH:12])[NH:8][C:7](=[O:14])[CH2:6][CH2:5]2.[OH-].[Na+].Br[CH2:18][CH2:19][CH2:20][Cl:21]>C(O)(C)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([Br:13])[C:11]=1[O:12][CH2:18][CH2:19][CH2:20][Cl:21])[NH:8][C:7](=[O:14])[CH2:6][CH2:5]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 80061-Bromo-3-chloropropaneHCID 14798Sodium HydroxideHCID 21243036HCID 21243036, 화합물

생성물 1

HCID 12899443HCID 12899443, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

5 grams of 6-chloro-8-bromo-7-hydroxy-3,4-dihydrocarbostyril and 3 g of sodium hydroxide are mixed with 120 ml of isopropanol and stirred at 50°-60° C. for 1 hour. Then 10 ml of 3-bromo-1-chloropropane are added thereto and stirred at 70°-80° C. for 6 hours. The reaction mixture is concentrated under reduced pressure to dryness and the residue thus obtained is extracted with chloroform. The chloroform layer is washed with water and dried. Then chloroform is removed by distillation and the residue thus formed is recrystallized from ethanol to obtain 6.2 g of 6-chloro-8-bromo-7-(3-chloropropoxy)-3,4-dihydrocarbostyril in the form of colorless needle-like crystals with a melting point of 87°-88° C.

후처리

  1. stirringstirred at 70°-80° C. for 6 hours
  2. concentrationThe reaction mixture is concentrated under reduced pressure to dryness
  3. customthe residue thus obtained
  4. extractionis extracted with chloroform
  5. washThe chloroform layer is washed with water
  6. customdried
  7. customThen chloroform is removed by distillation
  8. customthe residue thus formed
  9. customis recrystallized from ethanol

출처 및 근거

ORD 기록
ord-e09a748330134ccc891cc652b2bc3323
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04824840

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