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Sodium Iodide → 6'-methoxy-5',7'-dimethyl-1'-(quinolin-2-ylmethyl)-3',4'-dihydro-1'H-spiro[cyclobutane-1,2'-quinoline]

HRID 2103088
ノート
印刷プレビュー

反応式

HRID 2103088 の反応式
[CH3:1][O:2][C:3]1[C:4]([CH3:17])=[C:5]2[C:10](=[CH:11][C:12]=1[CH3:13])[NH:9][C:8]1([CH2:16][CH2:15][CH2:14]1)[CH2:7][CH2:6]2.Cl[CH2:19][C:20]1[CH:29]=[CH:28][C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[N:21]=1.C([O-])([O-])=O.[K+].[K+].[I-].[Na+]>CC(C)=O>[CH3:1][O:2][C:3]1[C:4]([CH3:17])=[C:5]2[C:10](=[CH:11][C:12]=1[CH3:13])[N:9]([CH2:19][C:20]1[CH:29]=[CH:28][C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[N:21]=1)[C:8]1([CH2:14][CH2:15][CH2:16]1)[CH2:7][CH2:6]2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 203942-(Chloromethyl)quinolineHCID 578035566'-methoxy-5',7'-dimethyl-3',4'-dihydro-1'H-spiro[cyclobutane-1,2'-quinoline]

生成物 1

HCID 690595946'-methoxy-5',7'-dimethyl-1'-(quinolin-2-ylmethyl)-3',4'-dihydro-1'H-spiro[cyclobutane-1,2'-quinoline]収率 57.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 6′-methoxy-5′,7′-dimethyl-3′,4′-dihydro-1′H-spiro[cyclobutane-1,2′-quinoline] (270 mg), 2-(chloromethyl)quinoline (626 mg), K2CO3 (528 mg) and sodium iodide (30 mg) in acetone (20 mL) was refluxed over night. After evaporation of the solvent, water was added to the residue and the aqueous solution was extracted with ethyl acetate (3×20 mL). The combined organic layers were dried over Na2SO4 and the solvent was removed by evaporation. The residue was purified by column chromatography (10% ethyl acetate/hexane), giving 6′-methoxy-5′,7′-dimethyl-1′-(quinolin-2-ylmethyl)-3′,4′-dihydro-1′H-spiro[cyclobutane-1,2′-quinoline] as a light yellow solid (250 mg).

後処理

  1. temperaturewas refluxed over night
  2. customAfter evaporation of the solvent, water
  3. additionwas added to the residue
  4. extractionthe aqueous solution was extracted with ethyl acetate (3×20 mL)
  5. dry with materialThe combined organic layers were dried over Na2SO4
  6. customthe solvent was removed by evaporation
  7. customThe residue was purified by column chromatography (10% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-ff324bebcda14148aef9d5450dd3042d
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07576094B2

反応ノート

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