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Water → cis-2,6-Dimethyl-4-[6-(2-methyl-3-furanyl)-2-pyridinyl]morpholine

HRID 2278425
ノート
印刷プレビュー

反応式

HRID 2278425 の反応式
CC1(C)C(C)(C)OB([C:9]2[CH:13]=[CH:12][O:11][C:10]=2[CH3:14])O1.Br[C:17]1[N:22]=[C:21]([N:23]2[CH2:28][C@H:27]([CH3:29])[O:26][C@H:25]([CH3:30])[CH2:24]2)[CH:20]=[CH:19][CH:18]=1.O.C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1.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>[CH3:30][C@H:25]1[O:26][C@@H:27]([CH3:29])[CH2:28][N:23]([C:21]2[CH:20]=[CH:19][CH:18]=[C:17]([C:9]3[CH:13]=[CH:12][O:11][C:10]=3[CH3:14])[N:22]=2)[CH2:24]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 4

HCID 962WaterHCID 10340Sodium Carbonate2 回HCID 242295474,4,5,5-Tetramethyl-2-(2-methylfuran-3-yl)-1,3,2-dioxaborolane2 回HCID 86702423cis-4-(6-Bromo-2-pyridinyl)-2,6-dimethylmorpholine

生成物 1

HCID 67514523cis-2,6-Dimethyl-4-[6-(2-methyl-3-furanyl)-2-pyridinyl]morpholine

試薬・触媒・溶媒 3

HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 178418397HCID 178418397、化合物触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

4,4,5,5-Tetramethyl-2-(2-methyl-3-furanyl)-1,3,2-dioxaborolane (412 mg, 1.980 mmol) was added to a solution of cis-4-(6-bromo-2-pyridinyl)-2,6-dimethylmorpholine (537 mg, 1.980 mmol) in a mixture of 1,4-dioxane (15 mL), water (2.500 mL) and sodium carbonate (420 mg, 3.96 mmol). The solution was degassed using argon gas and then charged with tetrakis(triphenylphosphine)palladium(0) (229 mg, 0.198 mmol). After addition, the reaction mixture was stirred and heated in the microwave at 100° C. for 1 hour. Crude LC/MS showed starting material and desired product so tetrakis(triphenylphosphine) palladium(0) (229 mg, 0.198 mmol), sodium carbonate (420 mg, 3.96 mmol) and 4,4,5,5-tetramethyl-2-(2-methyl-3-furanyl)-1,3,2-dioxaborolane (412 mg, 1.980 mmol) were added to the reaction mixture which was then stirred and heated at 100° C. in the microwave for 1 hour. Crude LC/MS showed desired product and no starting material can be seen. The reaction mixture was washed with ethyl acetate (200 mL), water (100 mL), filtered and then evaporated to dryness. The residue was dissolved in dichloromethane (˜5 ml) and purified on silica by a Biotage SP4 chromatographic system (40+M cartridge, eluted with 0-50% ethyl acetate in isohexanes). Fractions containing pure product were combined and concentrated under reduced pressure to give the title compound as a colourless oil (270 mg, 0.942 mmol, 47.6% yield). LC/MS [M+H]+=273.

後処理

  1. customThe solution was degassed
  2. additionAfter addition

出典と根拠

ORDレコード
ord-6a1da768e85f4698848cdf14eb43ef0e
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133178B2

反応ノート

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