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Epichlorohydrin → HCID 12899440、化合物

HRID 1979763
ノート
印刷プレビュー

反応式

HRID 1979763 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([OH:13])=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8][CH2:7]2.C(=O)([O-])[O-].[K+].[K+].[CH2:20]([CH:22]1[O:24][CH2:23]1)Cl.[OH-].[Na+]>C(O)(C)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([O:13][CH2:20][CH:22]2[O:24][CH2:23]2)=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8][CH2:7]2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 7835EpichlorohydrinHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 12899415HCID 12899415、化合物

生成物 1

HCID 12899440HCID 12899440、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

20.0 Grams of 8-bromo-5-hydroxy-3,4-dihydrocarbostyril and 18 g of potassium carbonate were dispersed in 160 ml of isopropanol, then 40 ml of epichlorohydrin was added thereinto and reacted at 80° C. for 6 hours. The reaction mixture was concentrated under a reduced pressure and to the residue thus obtained was added 100 ml of 2N-sodium hydroxide and stirred well. The insoluble matters formed were obtained by filtration and washed with water and dried to obtain crude crystals. Recrystallization of the crude crystal from methanol to obtain 18.5 g of 8-bromo-5-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril as in the form of colorless needle-like crystals. Melting point: 220°-220° C.

後処理

  1. customreacted at 80° C. for 6 hours
  2. concentrationThe reaction mixture was concentrated under a reduced pressure and to the residue
  3. customthus obtained
  4. customThe insoluble matters formed
  5. customwere obtained by filtration
  6. washwashed with water
  7. customdried
  8. customto obtain crude crystals
  9. customRecrystallization of the crude crystal from methanol

出典と根拠

ORDレコード
ord-7f68d63a85dd4776989d5324d086d316
出典データセット
uspto-grants-1984_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04482560

反応ノート

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