Hydrazine hydrate (1:1) → alpha-Methylcyclohexaneethanamine

HRID 1277482ノート

反応式

HRID 1277482 の反応式
[CH:1]1([CH2:7][CH:8]([NH:10]C(=O)CN2C(=O)C3=CC=CC=C3C2=O)[CH3:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.O.NN>C(O)C>[NH2:10][CH:8]([CH3:9])[CH2:7][CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 23454125HCID 23454125、化合物

生成物 1

HCID 115665alpha-Methylcyclohexaneethanamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of (±)-N-(2-cyclohexyl-1-methylethyl)-2-phthalimidoacetamide (12.0 g, 36.7mmol) in ethanol (180 ml) was added hydrazine hydrate (2.05 g, 40.3 mmol) and the mixture heated under reflux for 1.5 hours. After cooling and standing at 0° for 24 hours, the slurry was filtered and the residue washed with petrol (40°-60°). The combined filtrateswere evaporated to dryness and the oily residue triturated with petrol (3×100 ml). The combined extracts were evaporated to dryness to givea colourless oil. The oil was dissolved in ether (50 ml) and the solution added to a warm solution of fumaric acid (2.7 g) in ethanol (50 ml). On standing, a colourless solid was deposited, m.p. 132°-134° C.

後処理

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 1.5 hours
  3. temperatureAfter cooling
  4. filtrationthe slurry was filtered
  5. washthe residue washed with petrol (40°-60°)
  6. customThe combined filtrateswere evaporated to dryness
  7. customthe oily residue triturated with petrol (3×100 ml)
  8. customThe combined extracts were evaporated to dryness
  9. dissolutionThe oil was dissolved in ether (50 ml)
  10. additionthe solution added to a warm solution of fumaric acid (2.7 g) in ethanol (50 ml)

出典と根拠

ORDレコード
ord-8d4e06da135243daafe82bb006255f54
出典データセット
uspto-grants-1981_07
特許番号
US04277498

反応ノート

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