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Cesium carbonate → ethyl 3-[4-({(tert-butoxycarbonyl)[(1R)-1-(1-naphthyl)ethyl]amino}methyl)-3-phenylpiperidin-1-yl]benzoate

HRID 1691730
ノート
印刷プレビュー

反応式

HRID 1691730 の反応式
O1CCOCC1.[C:7]([O:11][C:12](=[O:39])[N:13]([C@@H:27]([C:29]1[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[CH:32]=[CH:31][CH:30]=1)[CH3:28])[CH2:14][CH:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH:16]1[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)([CH3:10])([CH3:9])[CH3:8].I[C:41]1[CH:42]=[C:43]([CH:49]=[CH:50][CH:51]=1)[C:44]([O:46][CH2:47][CH3:48])=[O:45].C(=O)([O-])[O-].[Cs+].[Cs+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(P(C2CCCCC2)C2C=CC=CC=2C2C=CC=CC=2N(C)C)CCCCC1.C(OCC)(=O)C.C(O)(C)(C)C>[C:7]([O:11][C:12]([N:13]([CH2:14][CH:15]1[CH2:20][CH2:19][N:18]([C:41]2[CH:42]=[C:43]([CH:49]=[CH:50][CH:51]=2)[C:44]([O:46][CH2:47][CH3:48])=[O:45])[CH2:17][CH:16]1[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[C@@H:27]([C:29]1[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[CH:32]=[CH:31][CH:30]=1)[CH3:28])=[O:39])([CH3:8])([CH3:9])[CH3:10]
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 4

HCID 10796Cesium carbonateHCID 312751,4-Dioxane2 回HCID 143542Ethyl 3-iodobenzoateHCID 59178521HCID 59178521、化合物

生成物 1

HCID 66906240ethyl 3-[4-({(tert-butoxycarbonyl)[(1R)-1-(1-naphthyl)ethyl]amino}methyl)-3-phenylpiperidin-1-yl]benzoate収率 81%

試薬・触媒・溶媒 4

HCID 2734217
2-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenyl
触媒
HCID 9811564Bis(dibenzylideneacetone)palladium触媒
HCID 6386tert-Butanol溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

To a mixture of 2.3 mg of tris(dibenzylideneacetone)dipalladium(0), 1.9 mg of 2-(dicyclohexylphosphino)-2′-(dimethylamino)biphenyl, and 0.5 mL of 1,4-dioxane were added 100 mg of tert-butyl[(1R)-1-(1-naphthyl)ethyl][(3-phenylpiperidin-4-yl)methyl]carbamate, 83.8 mg of ethyl 3-iodobenzoate, 105 mg of cesium carbonate, 1.0 mL of 1,4-dioxane, and 1.5 mL of t-butanol, followed by stirring at 100° C. overnight. After cooling to room temperature, to the reaction mixture was added ethyl acetate, the insolubles were removed, and the solvent was removed by distillation under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 108 mg of ethyl 3-[4-({(tert-butoxycarbonyl)[(1R)-1-(1-naphthyl)ethyl]amino}methyl)-3-phenylpiperidin-1-yl]benzoate as a pale yellow foamy substance. ESI+: 593

後処理

  1. temperatureAfter cooling to room temperature, to the reaction mixture
  2. customthe insolubles were removed
  3. customthe solvent was removed by distillation under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-73d9afbf22ea4b9b8363dc939f337a8d
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08153658B2

反応ノート

読み込み中…

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