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Hydrazine hydrate (1:1) → 2-Hydroxy-3-[3-(1-piperidylmethyl)benzyloxy]propylamine

HRID 542199
ノート
印刷プレビュー

反応式

HRID 542199 の反応式
[OH:1][CH:2]([CH2:15][O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([CH2:24][N:25]2[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]2)[CH:19]=1)[CH2:3][N:4]1C(=O)C2C(=CC=CC=2)C1=O.O.NN>C(O)C>[OH:1][CH:2]([CH2:15][O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([CH2:24][N:25]2[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]2)[CH:19]=1)[CH2:3][NH2:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 135354762-[2-Hydroxy-3-[3-(1-piperidylmethyl)benzyloxy]propyl]-1H-isoindole-1,3-dione

生成物 1

HCID 135354772-Hydroxy-3-[3-(1-piperidylmethyl)benzyloxy]propylamine収率 76%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

8.60 g (0.021 mol) of 2-[2-hydroxy-3-[3-(1-piperidylmethyl)-benzyloxy]propyl]-1H-isoindole-1,3-dione and 3.3 ml of hydrazine hydrate (80%) are boiled in 80 ml of ethanol for 3 hours. The residdue left after concentration of the mixture by evaporation is taken up in 50 ml of water; 8 ml of conc. hydrochloric acid are added and the reaction mixture is filtered. The filtrate is adjusted to pH 12 with conc. sodium hydroxide solution and extracted with 3×40 ml methylene chloride. The organic phase is dehydrated with Na2SO4 and concentrated by evaporation under vacuum. The residue is distilled in a high vacuum. 4.44 g (76%) of a colourless oil, boiling point 145°-155° C./1×10-2 mbar are obtained. ##STR4##

後処理

  1. waitThe residdue left after concentration of the mixture
  2. customby evaporation
  3. addition8 ml of conc. hydrochloric acid are added
  4. filtrationthe reaction mixture is filtered
  5. extractionextracted with 3×40 ml methylene chloride
  6. concentrationconcentrated by evaporation under vacuum
  7. distillationThe residue is distilled in a high vacuum

出典と根拠

ORDレコード
ord-8e86cb543b544a38bf75606f073c6257
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04656180

反応ノート

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