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Sodium Carbonate → HCID 11280481、化合物

HRID 2216313
ノート
印刷プレビュー

反応式

HRID 2216313 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[C:14]([CH3:15])=[CH:13][C:12]([CH3:16])=[CH:11][C:10]=2[CH3:17])[C:5]([S:18]([C:21]2[CH:26]=[CH:25][C:24](OS(C(F)(F)F)(=O)=O)=[CH:23][CH:22]=2)(=[O:20])=[O:19])=[CH:4][N:3]=1.[CH3:35]B(O)O.C([O-])([O-])=O.[Na+].[Na+].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.COCCOC>[CH3:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[C:14]([CH3:15])=[CH:13][C:12]([CH3:16])=[CH:11][C:10]=2[CH3:17])[C:5]([S:18]([C:21]2[CH:26]=[CH:25][C:24]([CH3:35])=[CH:23][CH:22]=2)(=[O:20])=[O:19])=[CH:4][N:3]=1
参加物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 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 139377Methylboronic AcidHCID 86595018HCID 86595018、化合物

生成物 1

HCID 11280481HCID 11280481、化合物収率 65.1%

試薬・触媒・溶媒 3

HCID 178418476
HCID 178418476、化合物
触媒
HCID 962Water溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

A mixture of trifluoromethanesulfonic acid 4-[2-methyl-4-(2,4,6-trimethylphenylamino)-pyrimidine-5-sulfonyl]-phenyl ester (158 mg, 0.306 mmol), prepared by the method described in Example 22, methylboronic acid (36 mg, 0.61 mmol), 2 M Na2CO3 (2.0 mL, 4.0 mmol), and DME (4 mL) was degassed with N2 for 10 min, and then PdCl2(PPh3)2 (43 mg, 0.061 mmol) and triphenylphosphine (32 mg, 0.12 mmol) were added. The mixture was refluxed under N2 for 2 h and then cooled to room temperature. The reaction mixture was diluted with water, and extracted (3×) with EtOAc. The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by chromatography on silica gel (67:33 hexanes/EtOAc) to provide the desired product (76 mg, 65%) as a white solid: mp 202–204° C.; 1H NMR (300 MHz, CDCl3) δ 8.75 (s, 1H), 8.23 (br s, 1H), 7.84 (d, J=8.4 Hz, 2H), 7.33 (d, J=8.4 Hz, 2H), 6.91 (s, 2H), 2.43 (s, 3H), 2.38 (s, 3H), 2.30 (s, 3H), 2.00 (s, 6H); ESI MS m/z 382 [(M+H)+, calcd for C21H24N3O2S, 382.2].

後処理

  1. customprepared by the method
  2. customwas degassed with N2 for 10 min
  3. temperatureThe mixture was refluxed under N2 for 2 h
  4. extractionextracted (3×) with EtOAc
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by chromatography on silica gel (67:33 hexanes/EtOAc)

出典と根拠

ORDレコード
ord-9aad94727db841ff8c8a1ebcfb1e4c99
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07112585B2

反応ノート

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