(5-Nitro-2-sulfanylphenyl)methanol → HCID 19045546、化合物

HRID 1591176ノート

反応式

HRID 1591176 の反応式
[SH:1][C:2]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:3]=1[CH2:4][OH:5].N1C=CC=CC=1[CH2:19][CH2:20][CH:21]1[CH2:26][C:25](=O)[CH2:24][CH2:23][NH:22]1>C(Cl)(Cl)Cl>[N+:10]([C:7]1[CH:8]=[CH:9][C:2]2[S:1][C:25]3([CH2:24][CH2:23][N:22]([CH2:19][CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=4)[CH2:21][CH2:26]3)[O:5][CH2:4][C:3]=2[CH:6]=1)([O-:12])=[O:11]

参加物

4

反応物 2

HCID 54329580(5-Nitro-2-sulfanylphenyl)methanolHCID 86746766HCID 86746766、化合物

生成物 1

HCID 19045546HCID 19045546、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
25 °C

実験手順

2-Mercapto-5-nitrobenzyl alcohol (150 mg, 0.81 mmol) and 208 mg (0.80 mm) of N-[2-(2'-pyridylethyl]-4-piperidone was dissolved in 5 mL of CHCl3. HCl Gas was bubbled in to saturate the solution, the mixture stirred at 25° C. for 2 days, then diluted with water and the pH adjusted to 10.0 with 40% aqueous NaOH. Extraction with CHCl3 and drying the organic phase (Na2SO4) gave after concentration and recrystallization from ethyl acetate 75 mg of an orange solid.

後処理

  1. customHCl Gas was bubbled in
  2. concentrationto saturate the solution
  3. additiondiluted with water
  4. extractionExtraction with CHCl3
  5. dry with materialdrying the organic phase (Na2SO4)
  6. customgave
  7. concentrationafter concentration and recrystallization from ethyl acetate 75 mg of an orange solid

出典と根拠

ORDレコード
ord-1a2810c8769c4e04add6d2d2b90ec0db
出典データセット
uspto-grants-1993_04
特許番号
US05206240

反応ノート

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