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1-Bromo-3-chloropropane → HCID 12899443、化合物

HRID 621553
ノート
印刷プレビュー

反応式

HRID 621553 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 80061-Bromo-3-chloropropaneHCID 14798Sodium HydroxideHCID 21243036HCID 21243036、化合物

生成物 1

HCID 12899443HCID 12899443、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e09a748330134ccc891cc652b2bc3323
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04824840

反応ノート

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