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

HRID 19728노트

반응식

HRID 19728 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6701d69aee314211944330f445d96ad7
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745462B2

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