Delta-Valerolactone → HCID 12365950、化合物

HRID 2398047

反応式

HRID 2398047 の反応式
[C:1]1(=O)O[CH2:5][CH2:4][CH2:3][CH2:2]1.S(Cl)(Cl)=O.ClC(C)CCC(Cl)=O.[Cl:20][C:21]1[CH:30]=[C:25]([C:26]([NH:28][OH:29])=[O:27])[C:24]([OH:31])=[CH:23][CH:22]=1>[Cl-].[Zn+2].[Cl-]>[Cl:20][C:21]1[CH:22]=[CH:23][C:24]2[O:31][CH:1]3[CH2:2][CH2:3][CH:4]([CH3:5])[O:29][N:28]3[C:26](=[O:27])[C:25]=2[CH:30]=1

参加物

6

反応物 4

HCID 10953Delta-ValerolactoneHCID 24386Thionyl ChlorideHCID 169935Benzamide, 5-chloro-N,2-dihydroxy-HCID 126039624-Chloropentanoyl chloride

生成物 1

HCID 12365950HCID 12365950、化合物

試薬・触媒・溶媒 1

HCID 3007855Zincchloride触媒

実験手順

A mixture of 30 g. of γ -valerolactone, 30 ml. of distilled thionyl chloride and 0.5 g. of zinc chloride was heated on a steam bath overnight and then distilled at 15 mm. The distillate was redistilled at 69- 70° and 15 mm. giving 34 g. of 4-chlorovaleryl chloride. The acid chloride was reduced catalytically, reacted with 5-chlorosalicylhydroxamic acid and the resulting intermediate was ring-closed according to the method described in Example 3. The product after recrystallization from trichloroethylene weighed 8.5 g. and melted at 210- 213° C.

後処理

  1. additionA mixture of 30 g
  2. distillationdistilled at 15 mm
  3. distillationThe distillate was redistilled at 69- 70°
  4. customgiving 34 g
  5. customthe resulting intermediate was ring-closed
  6. customThe product after recrystallization from trichloroethylene

出典と根拠

ORDレコード
ord-c9f79d7b0bf3447899fe351abbbcff38
出典データセット
uspto-grants-1977_05
特許番号
US04024139

関連ノート

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