Dichloromethane → HCID 10382997、化合物

HRID 1352495ノート

反応式

HRID 1352495 の反応式
[CH3:1][CH:2]1[CH2:11][CH:10]([NH:12][CH2:13][C:14]#[CH:15])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]1[C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:17].C(N([CH:30]([CH3:32])C)CC)(C)C.ClCCl.C(=O)([O-])[O-:37].[K+].[K+]>O1CCOCC1>[C:16]([N:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH:10]([N:12]([CH2:13][C:14]#[CH:15])[C:30](=[O:37])[CH3:32])[CH2:11][CH:2]1[CH3:1])(=[O:17])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 22935713HCID 22935713、化合物

生成物 1

HCID 10382997HCID 10382997、化合物収率 58.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of (2-methyl-4-prop-2-ynylamino-3,4-dihydro-2H-quinolin-1-yl)-phenyl-methanone (0.06 g), diisopropyl ethyl amine (0.038 g) in dioxane (5 ml), anhydride acetic (0.2 g) was added under stirring. The mixture was heated under reflux over the night. After cooling dichloromethane and an aqueous solution of potassium carbonate were added. The organic layer was separated, and then dried over sodium sulfate. Organic solvent was removed under reduce pressure to give the crude compound (0.15 g). Purification by chromatography was performed with dichloromethane/methanol (99/1) as eluent to give the desired title compound (0.04 g, 58.8% yield).

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux over the night
  3. customThe organic layer was separated
  4. dry with materialdried over sodium sulfate
  5. customOrganic solvent was removed
  6. customto give the crude compound (0.15 g)
  7. customPurification by chromatography

出典と根拠

ORDレコード
ord-794b2bf971e7467ca02c7291e8721d69
出典データセット
uspto-grants-2007_05
特許番号
US07220760B2

反応ノート

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