Phenol → 11-Phenoxy-1,2,4,5-tetrahydro-3-azepino[4,5-b]quinoline-carboxylic acid ethyl ester

HRID 1288187ノート

反応式

HRID 1288187 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]=2Cl)[CH2:8][CH2:7]1)=[O:5])[CH3:2].[C:22]1([OH:28])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(OCC)(=O)C>[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[O:28][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:8][CH2:7]1)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 996PhenolHCID 2150364411-chloro-3-ethoxycarbonyl-1,2,4,5-tetrahydro-3H-azepino[4,5-b]quinoline

生成物 1

HCID 5423109711-Phenoxy-1,2,4,5-tetrahydro-3-azepino[4,5-b]quinoline-carboxylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 15.0 gm (49.4 millimols) of 11-chloro-1,2,4,5-tetrahydro-3-azepino[4,5-b]quinoline-carboxylic acid ethyl ester and 28.2 gm (300 millimols) of phenol was melted at 150° C and held at that temperature for 40 hours. Then, the mixture was taken up in ethyl acetate, and the solution was extracted with dilute sodium hydroxide. The ethyl acetate phases were evaporated and chromatographed on a silicagel column with toluene/acetone (8:1) as the eluant. Subsequently, the crystals were triturated with ether/petroleum ether.

後処理

  1. extractionthe solution was extracted with dilute sodium hydroxide
  2. customThe ethyl acetate phases were evaporated
  3. customchromatographed on a silicagel column with toluene/acetone (8:1) as the eluant
  4. customSubsequently, the crystals were triturated with ether/petroleum ether

出典と根拠

ORDレコード
ord-dfe7b2acd7bb4ce0995ab0bb82a780ae
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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