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Potassium Carbonate → methyl (R)-2-tert-butoxycarbonylamino-3-(3'-formylbiphenyl-4-yl)propionate

HRID 271857
ノート
印刷プレビュー

反応式

HRID 271857 の反応式
[C:1](=[O:4])([O-])[O-].[K+].[K+].[C:7]([O:11][C:12]([NH:14][C@H:15]([CH2:20][C:21]1[CH:26]=[CH:25][C:24](OS(C(F)(F)F)(=O)=O)=[CH:23][CH:22]=1)[C:16]([O:18][CH3:19])=[O:17])=[O:13])([CH3:10])([CH3:9])[CH3:8]>COCCOC.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[Pd]>[C:7]([O:11][C:12]([NH:14][C@H:15]([CH2:20][C:21]1[CH:26]=[CH:25][C:24]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([CH:1]=[O:4])[CH:22]=2)=[CH:23][CH:22]=1)[C:16]([O:18][CH3:19])=[O:17])=[O:13])([CH3:10])([CH3:9])[CH3:8]
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

5

反応物 2

HCID 11430Potassium CarbonateHCID 53983472(R)-methyl 2-((tert-butoxycarbonyl)amino)-3-(4-(((trifluoromethyl)sulfonyl)oxy)phenyl)propanoate

生成物 1

HCID 86601623methyl (R)-2-tert-butoxycarbonylamino-3-(3'-formylbiphenyl-4-yl)propionate収率 35%

試薬・触媒・溶媒 2

HCID 178527696HCID 178527696、化合物触媒
HCID 8071
1,2-Dimethoxyethane
溶媒

反応条件

温度
85 °C

実験手順

100 ml (201 mmol) of an aqueous 2M potassium carbonate solution and 4.4 g (3.80 mmol) of tetrakis palladium are introduced into a solution containing 33 g (77.3 mmol) of methyl (R)-2-tert-butoxycarbonylamino-3-(4-trifluoromethanesulfonyloxyphenyl)propionate, and 15 g (100 mmol) of 3-boronic acid-benzaldehyde (Example 28b) in 300 ml of ethylene glycol dimethyl ether. The reaction medium is heated at 85° C. for 20 h and, after a return to ambient temperature, extracted with ethyl acetate. The organic phase is washed with water and then a saturated sodium chloride solution, dried over magnesium sulfate, and concentrated. The residue obtained is purified by chromatography on a column of silica and eluted with a 7/3 heptane/ethyl acetate mixture. 10.2 g of coupled product are obtained with a 35% yield.

後処理

  1. extractionafter a return to ambient temperature, extracted with ethyl acetate
  2. washThe organic phase is washed with water
  3. dry with materiala saturated sodium chloride solution, dried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue obtained
  6. customis purified by chromatography on a column of silica
  7. washeluted with a 7/3 heptane/ethyl acetate mixture

出典と根拠

ORDレコード
ord-043578fe9d47433a91e8bf99c4dc3215
出典データセット
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07452878B2

反応ノート

読み込み中…

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