Diethyl Ether → HCID 10752374、化合物

HRID 345856ノート

反応式

HRID 345856 の反応式
[I-].[C:2]1([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][CH2:10][N+:9]=2[CH3:18])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:19](OCC)C.C[Mg]Br.[Cl-].[NH4+]>O1CCCC1.C(OCC)(=O)C>[CH3:19][C:8]1([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][N:9]1[CH3:18]

参加物

7

反応物 4

HCID 3283Diethyl EtherHCID 25517Ammonium ChlorideHCID 10521731HCID 10521731、化合物HCID 178418573HCID 178418573、化合物

生成物 1

HCID 10752374HCID 10752374、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a suspension of 1-phenyl-2-methyl-3,4-dihydroisoquinolinium iodide (1.0 g) in tetrahydrofuran (15 ml) was added 3M diethyl ether solution of methyl magnesium bromide (1.9 ml) with stirring at room temperature. After stirring for 30 minutes, the mixture was poured into saturated ammonium chloride aqueous solution and ethyl acetate. The organic layer was washed with water, sodium chloride aqueous solution and dried over magnesium sulfate, and evaporated in vacuo. The residue was recrystallized from n-hexane to give 1,2-dimethyl-1-phenyl-1,2,3,4-tetrahydroisoquinoline (0.6 g).

後処理

  1. stirringAfter stirring for 30 minutes
  2. washThe organic layer was washed with water, sodium chloride aqueous solution
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was recrystallized from n-hexane

出典と根拠

ORDレコード
ord-6c1441b1ac2a4f198b360c0d349df31c
出典データセット
uspto-grants-1991_10
特許番号
US05059608

反応ノート

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