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Aluminum(III) Chloride → 1,8-Dimethyl-1,2,3,4-tetrahydroisoquinoline

HRID 2293135
ノート
印刷プレビュー

反応式

HRID 2293135 の反応式
Cl.Br[CH2:3][CH2:4][NH:5][CH:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:14])[CH3:7].[Cl-].[Al+3].[Cl-].[Cl-]>C1C2C(CCCC2)CCC1>[CH3:7][CH:6]1[C:8]2[C:13](=[CH:12][CH:11]=[CH:10][C:9]=2[CH3:14])[CH2:3][CH2:4][NH:5]1
参加物反応条件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 6451240Aluminum(III) ChlorideHCID 21476474HCID 21476474、化合物

生成物 1

HCID 214765001,8-Dimethyl-1,2,3,4-tetrahydroisoquinoline収率 37.1%

試薬・触媒・溶媒 1

HCID 7044Decalin溶媒

反応条件

温度
0 °C

実験手順

To a mixed solution of 14.7 g of the compound (45.5 mM) prepared in Step 4 above and 100 ml of decaline, was added aluminium chloride and reacted at 140°-150° C. for 1.5 hours, which was cooled to 0° C. The reaction mixture was diluted by pouring into ice water and washed with ethyl ether. The reaction mixture was basified by adding aqueous NaOH solution and the solids produced were filtered. The filtrate was extracted from ethyl ether and the extracts was dried over anhydrous sodium sulfate, concentrated under a reduced pressure, to give 3.16 g of the title compound.

後処理

  1. customreacted at 140°-150° C. for 1.5 hours
  2. additionThe reaction mixture was diluted
  3. washwashed with ethyl ether
  4. additionby adding aqueous NaOH solution
  5. customthe solids produced
  6. filtrationwere filtered
  7. extractionThe filtrate was extracted from ethyl ether
  8. dry with materialthe extracts was dried over anhydrous sodium sulfate
  9. concentrationconcentrated under a reduced pressure

出典と根拠

ORDレコード
ord-531df4841b654e1e91d04de2aba01087
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05686458

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート