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Hydrazine hydrate (1:1) → 6-(2-Methyl-1,3-dioxolan-2-yl)hexan-1-amine

HRID 1164496
ノート
印刷プレビュー

反応式

HRID 1164496 の反応式
[CH3:1][C:2]1([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]2C(=O)C3=CC=CC=C3C2=O)[O:6][CH2:5][CH2:4][O:3]1.O.NN>C(O)C>[CH3:1][C:2]1([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][NH2:13])[O:3][CH2:4][CH2:5][O:6]1
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 20511312N-[6-(2-Methyl-1,3-dioxolan-2-yl)hexyl]phthalimide

生成物 1

HCID 130938726-(2-Methyl-1,3-dioxolan-2-yl)hexan-1-amine収率 64%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 125.25 g (0.395 mole) of N-[6-(2-methyl-1,3-dioxolan-2-yl)hexyl]phthalimide, 23 ml of 85% hydrazine hydrate, and 370 ml of 95% ethanol was refluxed for four hours, cooled, filtered and stripped. The residue was mixed with 500 ml of water, basified with 2 N NaOH solution and extracted with methylene chloride. The organic layer was separated, dried over anhydrous potassium carbonate, filtered, and stripped to an orange oil. This material was distilled to give 35.70 g (64%) of clear oil bp 80°-83° (0.100 mm).

後処理

  1. temperaturewas refluxed for four hours
  2. temperaturecooled
  3. filtrationfiltered
  4. additionThe residue was mixed with 500 ml of water
  5. extractionextracted with methylene chloride
  6. customThe organic layer was separated
  7. dry with materialdried over anhydrous potassium carbonate
  8. filtrationfiltered
  9. distillationThis material was distilled

出典と根拠

ORDレコード
ord-82eb6438fb3043a6a2c519dfd2fb909c
出典データセット
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04370335

反応ノート

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