Diethyl Ether → HCID 10752374, 화합물

HRID 345856노트

반응식

HRID 345856 반응식
[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]

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 25517Ammonium ChlorideHCID 10521731HCID 10521731, 화합물HCID 178418573HCID 178418573, 화합물

생성물 1

HCID 10752374HCID 10752374, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6c1441b1ac2a4f198b360c0d349df31c
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05059608

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