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Aluminium lithium hydride → N-methyl-1,2,3,4-tetrahydronaphthalen-2-amine

HRID 1646225
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HRID 1646225 반응식
[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH:2]1[NH:11][C:12](OCC1C=CC=CC=1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[CH3:12][NH:11][CH:2]1[CH2:3][CH2:4][C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH2:1]1
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참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 54429858Phenylmethyl 1,2,3,4-tetrahydronaphthalene-2-carbamate

생성물 1

HCID 13579644N-methyl-1,2,3,4-tetrahydronaphthalen-2-amine수율 112.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

7.43 g (26.4 mmol) of phenylmethyl 1,2,3,4-tetrahydronaphthalene-2-carbamate were added in portions to a suspension of 4.5 g (26.4 mmol) of lithium aluminium hydride in 200 ml of tetrahydrofuran and the mixture was heated to reflux for 3 h 30, allowed to cool, and hydrolysed with an excess of aqueous 1N sodium hydroxide solution, the mixture was filtered and concentrated, and the residue was distilled at about 80 Pa between 140 and 240° C. 4.78 g of impure oil were obtained, which was utilised in its impure state in the following step.

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후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 3 h 30
  3. temperatureto cool
  4. filtrationhydrolysed with an excess of aqueous 1N sodium hydroxide solution, the mixture was filtered
  5. concentrationconcentrated
  6. distillationthe residue was distilled at about 80 Pa between 140 and 240° C

출처 및 근거

ORD 기록
ord-d8195d5b7dda4d5c8f0f31c082dfd204
출처 데이터셋
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05179108

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