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Hydrochloric Acid → 3-((1-Ethylpropyl)amino)-6-methyl-2,4-dinitrobenzyl alcohol

HRID 1577485
ノート
印刷プレビュー

反応式

HRID 1577485 の反応式
C([O:4][CH2:5][C:6]1[C:11]([CH3:12])=[CH:10][C:9]([N+:13]([O-:15])=[O:14])=[C:8]([NH:16][CH:17]([CH2:20][CH3:21])[CH2:18][CH3:19])[C:7]=1[N+:22]([O-:24])=[O:23])(=O)C.Cl.O>CO>[CH2:18]([CH:17]([NH:16][C:8]1[C:7]([N+:22]([O-:24])=[O:23])=[C:6]([C:11]([CH3:12])=[CH:10][C:9]=1[N+:13]([O-:15])=[O:14])[CH2:5][OH:4])[CH2:20][CH3:21])[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 129407633-[(1-Ethylpropyl)amino]-6-methyl-2,4-dinitrobenzyl acetate

生成物 1

HCID 1566883-((1-Ethylpropyl)amino)-6-methyl-2,4-dinitrobenzyl alcohol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A sample of 3-[(1-ethylpropyl)amino]-6-methyl-2,4-dinitrobenzyl acetate (23.1 g; 0.068 mol) is added to a mixture of concentrated hydrochloric acid (30 ml), water (40 ml) and methanol (320 ml). The reaction mixture is refluxed for 4 hours, cooled down and concentrated in vacuo. It is then diluted with water, extracted with ether, and the ether layer dried. The ether is removed in vacuo to leave a red oil, which readily solidifies to a yellow-orange solid (19.9 g; 98.5%). A similarly prepared and purified sample has a melting point of 51°-54° C.

後処理

  1. temperatureThe reaction mixture is refluxed for 4 hours
  2. temperaturecooled down
  3. concentrationconcentrated in vacuo
  4. additionIt is then diluted with water
  5. extractionextracted with ether
  6. dry with materialthe ether layer dried
  7. customThe ether is removed in vacuo
  8. customto leave a red oil, which
  9. customA similarly prepared
  10. custompurified sample

出典と根拠

ORDレコード
ord-5d83b8539f184fda89fc8be8dd7b8a25
出典データセット
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04288385

反応ノート

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