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Cesium carbonate → HCID 10226975、化合物

HRID 2416636
ノート
印刷プレビュー

反応式

HRID 2416636 の反応式
Br[C:2]1[CH:3]=[C:4]([C:8]2[O:12][N:11]=[C:10]3[CH:13]=[CH:14][C:15]([C:17]4[CH:22]=[CH:21][N:20]=[C:19]([NH:23][C:24](=[O:26])[CH3:25])[N:18]=4)=[CH:16][C:9]=23)[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[CH3:33][O:34][C:35]1[N:40]=[CH:39][C:38]([O:41][CH3:42])=[C:37](B(O)O)[N:36]=1.C(P(C(C)(C)C)C(C)(C)C)(C)(C)C>CN(C=O)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1C=CC=CC=1>[CH3:33][O:34][C:35]1[N:40]=[C:39]([C:2]2[CH:3]=[C:4]([C:8]3[O:12][N:11]=[C:10]4[CH:13]=[CH:14][C:15]([C:17]5[CH:22]=[CH:21][N:20]=[C:19]([NH:23][C:24](=[O:26])[CH3:25])[N:18]=5)=[CH:16][C:9]=34)[CH:5]=[CH:6][CH:7]=2)[C:38]([O:41][CH3:42])=[CH:37][N:36]=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 10796Cesium carbonateHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 22632293HCID 22632293、化合物HCID 22632309(2,5-Dimethoxypyrimidin-4-yl)boronic acid

生成物 1

HCID 10226975HCID 10226975、化合物収率 13%

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 241Benzene溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A flask was charged with N-{4-[3-(3-bromophenyl)-benzo[c]isoxazol-5-yl]-pyrimidin-2-yl}-acetamide (100 mg, 0.272 mmol), cesium carbonate (97.7 mg, 0.328 mmol), and 2,5-dimethoxypyrimidine-6-boronic acid (55.0 mg, 0.3 mmol). The flask was evacuated and back-filled with nitrogen 5-7 times before adding 5 mL of degassed p-dioxane and 1 mL of degassed DMF. To this stirring solution/suspension was added, 125 μL of a 10% w/v benzene solution of tri-tertbutylphosphine followed by the addition of Pd2(dba)3 (25 mg, 0.0272 mmol) slurred in 1 mL of degassed DMF. The reaction was stirred under nitrogen atmosphere, at 80° C. Reaction was followed by HPLC and deemed to be complete in 4 hours. The reaction mixture was suction filtered hot through a pad of diatomaceous earth and washed the precipitate with DMF and acetonitrile. The filtrate was reduced to an oil under reduced pressure and the crude material purified via HPLC utilizing acetonitrile/water/TFA as the eluent. The material was isolated as a bright yellow powder (15 mg, 13% yield). 1H NMR (500 MHz DMSO-d6) δ 8.93 (s, 1H) 8.6 (s, 1H), 8.31 (s, 1H), 8.29 (d, 1H), 8.25 (d, 1H), 8.07 (d, 1H), 7.87 (d, 1H), 7.81 (d, 1H), 7.77 (m, 1H), 4.02 (2 close sing, 6H) in ppm. LC-MS (ES+) m/e=469 (M+H)

後処理

  1. customThe flask was evacuated
  2. additionback-filled with nitrogen 5-7 times
  3. additionbefore adding 5 mL of degassed p-dioxane and 1 mL of degassed DMF
  4. additionTo this stirring solution/suspension was added
  5. customReaction
  6. filtrationfiltered hot through a pad of diatomaceous earth
  7. washwashed the precipitate with DMF and acetonitrile
  8. customthe crude material purified via HPLC

出典と根拠

ORDレコード
ord-e218a46ff184455aa014c4ab6c0e6a4f
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06825190B2

反応ノート

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