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

HRID 327026
ノート
印刷プレビュー

反応式

HRID 327026 の反応式
[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
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 21226445Aluminium lithium hydrideHCID 54429858Phenylmethyl 1,2,3,4-tetrahydronaphthalene-2-carbamate

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-b3239afd700e47c39a0af1e6bb6e6498
出典データセット
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05272157

反応ノート

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