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Phenylboronic Acid → 1-tert-butyl-5-(2-phenylpyrimidin-4-yl)-1H-pyrazole-3-carboxamide

HRID 925413
ノート
印刷プレビュー

反応式

HRID 925413 の反応式
[C:1]([N:5]1[C:9]([C:10]2[CH:15]=[CH:14][N:13]=[C:12](SC)[N:11]=2)=[CH:8][C:7]([C:18]([NH2:20])=[O:19])=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[C:21]1(B(O)O)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C1COCC1.S1C=CC=C1C([O-])=O.[Cu+2].S1C=CC=C1C([O-])=O.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>[C:1]([N:5]1[C:9]([C:10]2[CH:15]=[CH:14][N:13]=[C:12]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[N:11]=2)=[CH:8][C:7]([C:18]([NH2:20])=[O:19])=[N:6]1)([CH3:4])([CH3:3])[CH3:2]
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 2

HCID 66827Phenylboronic AcidHCID 665582581-tert-butyl-5-[2-(methylsulfanyl)pyrimidin-4-yl]-1H-pyrazole-3-carboxamide

生成物 1

HCID 665582631-tert-butyl-5-(2-phenylpyrimidin-4-yl)-1H-pyrazole-3-carboxamide収率 23%

試薬・触媒・溶媒 3

HCID 15171005Copper thiophene-2-carboxylate触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
130 °C

実験手順

50 mg (0.172 mmol) of 1-tert-butyl-5-[2-(methylsulfanyl)pyrimidin-4-yl]-1H-pyrazole-3-carboxamide, 42 mg (0.343 mmol) of phenyl boronic acid, 98 mg (0.515 mmol) of copper thiophencarboxylate and 20 mg (0.017 mmol) of palladium tetrakis were suspended in 1.5 mL of dry THF under argon atmosphere. The resulting suspension was heated a 130° C. for 1 h by microwave irradiation. The reaction mixture was then filtered on a silica plug, diluted with AcOEt and washed with aqueous NH4OH. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by preparative HPLC/MS to provide the title compound (23%).

後処理

  1. filtrationThe reaction mixture was then filtered on a silica plug
  2. additiondiluted with AcOEt
  3. washwashed with aqueous NH4OH
  4. washThe organic layer was washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by preparative HPLC/MS

出典と根拠

ORDレコード
ord-9519fee0745e4a598eabea785ad7b1ed
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09284298B2

反応ノート

読み込み中…

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