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Benzoyl Peroxide → 2-[1-(4,4-Difluorocyclohexyl)piperidin-4-yl]-5-chloro-7-iodo-2,3-dihydro-1H-isoindol-1-one

HRID 333217
ノート
印刷プレビュー

反応式

HRID 333217 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]([CH3:12])[C:5]([C:6]([O:8]C)=O)=[C:4]([I:13])[CH:3]=1.BrN1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.C(N(CC)CC)C.[F:47][C:48]1([F:61])[CH2:53][CH2:52][CH:51]([N:54]2[CH2:59][CH2:58][CH:57]([NH2:60])[CH2:56][CH2:55]2)[CH2:50][CH2:49]1>C(OC)(=O)C(C)(C)C.ClCCl.ClCCl.C(O)C>[F:61][C:48]1([F:47])[CH2:53][CH2:52][CH:51]([N:54]2[CH2:55][CH2:56][CH:57]([N:60]3[CH2:12][C:10]4[C:5](=[C:4]([I:13])[CH:3]=[C:2]([Cl:1])[CH:11]=4)[C:6]3=[O:8])[CH2:58][CH2:59]2)[CH2:50][CH2:49]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 7187Benzoyl Peroxide2 回HCID 8471TriethylamineHCID 67184N-bromobutanimide2 回HCID 67192903Methyl 4-chloro-2-iodo-6-methylbenzoateHCID 671942361-(4,4-Difluorocyclohexyl)-piperidin-4-ylamine

生成物 1

HCID 67193003
2-[1-(4,4-Difluorocyclohexyl)piperidin-4-yl]-5-chloro-7-iodo-2,3-dihydro-1H-isoindol-1-one
収率 46.9%

試薬・触媒・溶媒 3

HCID 6344Dichloromethane溶媒HCID 69027Methyl pivalate溶媒HCID 21584144Dichloromethane ethanol溶媒

反応条件

温度
85 °C

実験手順

To a solution of methyl 4-chloro-2-iodo-6-methylbenzoate (175 mg, 0.56 mmol) in methyl pivalate (1 mL), N-bromosuccinimide (120 mg, 0.67 mmol) and benzoylperoxide (14 mg, 0.06 mmol) were added. The reaction mixture was stirred at 85° C. under nitrogen atmosphere for 3 hours. Additional N-bromosuccinimide (60 mg) and benzoylperoxide (7 mg) were added and stirring continued for 1 hour. Crude was filtered on Gooch and washed with toluene. Volatiles were evaporated and the residue was dissolved in acetonitrile (2 mL). Triethylamine (0.28 mL, 2 mmol) and 1-(4,4-difluorocyclohexyl)-piperidin-4-ylamine (110 mg, 0.5 mmol) were added and the reaction mixture was stirred at 90° C. for 4 hours. Crude was diluted with dichloromethane and washed with 15% ammonium hydroxide. Organic phase was dried over sodium sulfate, filtered and evaporated. Column chromatography (dichloromethane/ethanol:97/3) afforded title compound (116 mg, 45% yield).

後処理

  1. stirringstirring
  2. waitcontinued for 1 hour
  3. filtrationCrude was filtered on Gooch
  4. washwashed with toluene
  5. customVolatiles were evaporated
  6. dissolutionthe residue was dissolved in acetonitrile (2 mL)
  7. stirringthe reaction mixture was stirred at 90° C. for 4 hours
  8. washwashed with 15% ammonium hydroxide
  9. dry with materialOrganic phase was dried over sodium sulfate
  10. filtrationfiltered
  11. customevaporated

出典と根拠

ORDレコード
ord-a44219cb4dd24fd18ca9a0809ba587a4
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877944B2

反応ノート

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