Thionyl Chloride → HCID 54025343、化合物

HRID 1288166ノート

反応式

HRID 1288166 の反応式
[CH2:1]([O:3][C:4]([N:6]1[CH2:20][CH2:19][C:18]2[C:9](=[N:10][C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=3[C:17]=2[CH3:21])[CH:8](O)[CH2:7]1)=[O:5])[CH3:2].S(Cl)([Cl:25])=O>>[CH2:1]([O:3][C:4]([N:6]1[CH2:20][CH2:19][C:18]2[C:9](=[N:10][C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=3[C:17]=2[CH3:21])[CH:8]([Cl:25])[CH2:7]1)=[O:5])[CH3:2]

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 53875304HCID 53875304、化合物

生成物 1

HCID 54025343HCID 54025343、化合物

実験手順

1 gm (3.3 millimols) of 5-hydroxy-1,2,4,5-tetrahydro-11methyl-3-azepino[4,5-b]quinoline-carboxylic acid ethyl ester was stirred for 2 hours with 20 ml of thionyl chloride at room temperature. The excess thionyl chloride was then distilled off in vacuo, the residue was dissolved in chloroform, the solution was dried with sodium sulfate, and the solvent was distilled off. After purification of the residue on a silicagel column with benzene/ethyl acetate (8:2) as the eluant, the yield was 0.55 gm (52% of theory), m.p. 131° C.

後処理

  1. distillationThe excess thionyl chloride was then distilled off in vacuo
  2. dissolutionthe residue was dissolved in chloroform
  3. dry with materialthe solution was dried with sodium sulfate
  4. distillationthe solvent was distilled off
  5. customAfter purification of the residue on a silicagel column with benzene/ethyl acetate (8:2) as the eluant

出典と根拠

ORDレコード
ord-9adbbbdbf2a241d3aad2826b7091c370
出典データセット
uspto-grants-1976_10
特許番号
US03987047

反応ノート

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