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Sodium Carbonate → HCID 117993486、化合物

HRID 922589
ノート
印刷プレビュー

反応式

HRID 922589 の反応式
Cl[C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([C@@:10]2([CH3:16])[CH2:14][CH2:13][NH:12][C:11]2=[O:15])=[CH:4][CH:3]=1.[CH3:17][N:18]1[C:26]2[C:21](=[CH:22][C:23](B(O)O)=[CH:24][CH:25]=2)[CH:20]=[CH:19]1.C([O-])([O-])=O.[Na+].[Na+]>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].O1CCOCC1>[CH3:9][O:8][C:6]1[C:5]([C@@:10]2([CH3:16])[CH2:14][CH2:13][NH:12][C:11]2=[O:15])=[CH:4][CH:3]=[C:2]([C:23]2[CH:22]=[C:21]3[C:26](=[CH:25][CH:24]=2)[N:18]([CH3:17])[CH:19]=[CH:20]3)[N:7]=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

6

反応物 3

HCID 10340Sodium CarbonateHCID 27598671-Methyl-1H-indole-5-boronic acidHCID 117992994(R)-3-(6-chloro-2-methoxypyridin-3-yl)-3-methylpyrrolidin-2-one

生成物 1

HCID 117993486HCID 117993486、化合物収率 99%

試薬・触媒・溶媒 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
110 °C

実験手順

To a vial was added (R)-3-(6-chloro-2-methoxypyridin-3-yl)-3-methylpyrrolidin-2-one (56.6 mg, 0.24 mmol) which was evaporated with dioxane (2.0 mL). 1-methyl-1H-indol-5-ylboronic acid (63.4 mg, 0.36 mmol) was next added followed by Pd(dppf)Cl2 (7.5 mg, 0.01 mmol). The mixture was sealed and degassed with nitrogen. Degassed dioxane (1.9 mL) and degassed 2 M Na2CO3 (0.27 mL, 2.3 equiv) were then added to the solid mixture. The reaction was stirred for 16 h at 110° C. The reaction was concentrated and partitioned between EtOAc/10% (w/v) aq. Na2CO3. The organic layer was washed with brine, dried over Na2SO4, and concentrated to provide a crude brown glass. Purification by column chromatography (4 g RediSep Gold column) with a 40-100% EtOAc/heptane gradient provided the title compound (78 mg, 99%) as a pale yellow glass. 1H NMR (600 MHz, CDCl3) δ: 1.62 (s, 3H), 2.10 (ddd, 1H), 2.67-2.76 (m, 1H), 3.37-3.47 (m, 2H), 3.82 (s, 3H), 4.10-4.12 (m, 3H), 5.59 (br. s., 1H), 6.56 (d, 1H), 7.07 (d, 1H), 7.34-7.39 (m, 2H), 7.67 (d, 1H), 7.92-7.96 (m, 1H), 8.30 (s, 1H); MS (AP+)(M+H) 336. The absolute stereochemistry was obtained via X-ray crystallographic analysis of single crystals obtained via crystallization from a mixture of DCM and EtOH. FIG. 2 is an ORTEP drawing of (R)-3-(2-methoxy-6-(1-methyl-H-indol-5-yl)pyridin-3-yl)-3-methylpyrrolidin-2-one.

後処理

  1. customwas evaporated with dioxane (2.0 mL)
  2. additionnext added
  3. customThe mixture was sealed
  4. customdegassed with nitrogen
  5. additionwere then added to the solid mixture
  6. concentrationThe reaction was concentrated
  7. custompartitioned between EtOAc/10% (w/v) aq. Na2CO3
  8. washThe organic layer was washed with brine
  9. dry with materialdried over Na2SO4
  10. concentrationconcentrated
  11. customto provide a crude brown glass
  12. customPurification by column chromatography (4 g RediSep Gold column) with a 40-100% EtOAc/heptane gradient

出典と根拠

ORDレコード
ord-2ceca911454f420b9589d2be75a8014e
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278953B2

反応ノート

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