Hydrazine hydrate (1:1) → 2-(methoxymethyl)-2,3-dihydro-1H-inden-2-amine

HRID 19728ノート

反応式

HRID 19728 の反応式
[CH3:1][O:2][CH2:3][C:4]1([N:13]2C(=O)C3C(=CC=CC=3)C2=O)[CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5]1.O.NN>C(O)C>[CH3:1][O:2][CH2:3][C:4]1([NH2:13])[CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)3 回HCID 685632312-(2-Methoxymethylindan-2-yl)-isoindole-1,3-dione

生成物 1

HCID 534076272-(methoxymethyl)-2,3-dihydro-1H-inden-2-amine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-(2-methoxymethylindan-2-yl)-isoindole-1,3-dione (0.30 g, 0.976 mmol) and hydrazine hydrate (47 μl, 0.976 mmol) in 95% ethanol (15 ml) is heated to reflux for 45 hours. Further hydrazine hydrate (9.4 μl, 0.976 mmol) is added and the reaction refluxed for an additional 16 hours, followed by addition of a final portion of hydrazine hydrate (9.4 μl, 0.976 mmol) and a further 16 hours reflux. After cooling, the resultant suspension is filtered and the filter cake washed with ethanol. The combined filtrate and washings are evaporated and triturated with ether to afford 2-methoxymethylindan-2-ylamine, MH+178.

後処理

  1. temperatureis heated
  2. temperatureto reflux for 45 hours
  3. temperaturethe reaction refluxed for an additional 16 hours
  4. temperaturea further 16 hours reflux
  5. temperatureAfter cooling
  6. filtrationthe resultant suspension is filtered
  7. washthe filter cake washed with ethanol
  8. customThe combined filtrate and washings are evaporated
  9. customtriturated with ether

出典と根拠

ORDレコード
ord-6701d69aee314211944330f445d96ad7
出典データセット
uspto-grants-2010_06
特許番号
US07745462B2

反応ノート

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