Dichloromethane → HCID 10382997, 화합물

HRID 1352495노트

반응식

HRID 1352495 반응식
[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

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 22935713HCID 22935713, 화합물

생성물 1

HCID 10382997HCID 10382997, 화합물수율 58.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-794b2bf971e7467ca02c7291e8721d69
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07220760B2

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