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Dimethyl Sulfoxide → HCID 12968706、化合物

HRID 1633538
ノート
印刷プレビュー

反応式

HRID 1633538 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH2:11][C:10]([C:22]2[CH:27]=[CH:26][C:25](OS(C(F)(F)F)(=O)=O)=[CH:24][CH:23]=2)([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH3:21])[CH:15]=2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CS(C)=[O:38].C(N(CC)CC)C.C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:76]([O:78][CH2:79]C)C>CO.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH3:76][O:78][C:79](=[O:38])[C:25]1[CH:24]=[CH:23][C:22]([C:10]2([C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH3:21])[CH:15]=3)[CH2:11][CH2:12][CH2:13][N:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH2:9]2)=[CH:27][CH:26]=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

8

反応物 5

HCID 679Dimethyl SulfoxideHCID 3283Diethyl EtherHCID 8471TriethylamineHCID 812191,3-Bis(diphenylphosphino)propaneHCID 12968705HCID 12968705、化合物

生成物 1

HCID 12968706HCID 12968706、化合物

試薬・触媒・溶媒 2

HCID 167845
palladium(II) acetate
触媒
HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

To a solution of trifluoro-methanesulfonic acid 4-[1-benzyl-3-(3-methoxy-phenyl)-piperidin-3-yl]-phenyl ester (12.9 g, 25.4 mmol) in a Parr pressure bottle in MeOH (39 mL) were added DMSO (18 mL) and triethylamine (21 mL, 151 mmol). To the reaction mixture were added palladium acetate (3.99 g, 17.8 mmol) and 1,3-bis (diphenylphosphino) propane (5.25 g, 12.3 mmol). The mixture was shaken under 40 psi of CO at 70° C. for 4 hours. The reaction mixture was cooled to room temperature and was diluted with diethyl ether (600 mL). The ether layer was washed with water (5×60 mL), dried (MgSO4) and concentrated. The crude residue was purified by flash chromatography with hexanes/EtOAc (3:1) to afford 9.82 g of 4-[1-benzyl-3-(3-methoxy-phenyl)-piperidin-3-yl]-benzoic acid methyl ester. 1HNMR (400 MHz, CDCl3) δ 7.87 (d, 2H), 7.41-7.20 (comp, 7H), 7.12 (t, 1H), 6.77 (s, 1H), 6.73(d, 1H) 6.66 (d, 1H), 3.86 (s, 3H), 3.71 (s, 3H), 3.51 (s, 2H), 3.05 (br, 1H), 2.68 (br, 1H), 2.55 (br, 1H), 2.41-2.24 (comp, 2H), 2.22-2.18 (m, 1H), 1.61-1.42 (comp, 2H); MS (M+1) 416.3.

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washThe ether layer was washed with water (5×60 mL)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customThe crude residue was purified by flash chromatography with hexanes/EtOAc (3:1)

出典と根拠

ORDレコード
ord-237ba27e45c04bdba90ab4c5b4776e83
出典データセット
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06503905B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート