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Cesium carbonate → HCID 136377184、化合物

HRID 1027304
ノート
印刷プレビュー

反応式

HRID 1027304 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([N:14]3[CH2:18][C@@H:17]4[CH2:19][N:20](C(OC(C)(C)C)=O)[CH2:21][C@@H:16]4[CH2:15]3)=[CH:10][CH:9]=2)=[C:4]([OH:29])[CH:3]=1.CC1(C)C(C)(C)OB([C:38]2[CH:39]=[N:40][N:41](C(OC(C)(C)C)=O)[CH:42]=2)O1.C([O-])([O-])=O.[Cs+].[Cs+].O1CCOCC1>CC(C1C=C(C(C)C)C(C2C(OC)=CC(Cl)=C(OC)C=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C.C1C=[C-]C(CCN)=CC=1.[Pd+2].O>[CH2:15]1[C@@H:16]2[CH2:21][NH:20][CH2:19][C@@H:17]2[CH2:18][N:14]1[C:11]1[N:12]=[N:13][C:8]([C:5]2[CH:6]=[CH:7][C:2]([C:38]3[CH:39]=[N:40][NH:41][CH:42]=3)=[CH:3][C:4]=2[OH:29])=[CH:9][CH:10]=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

7

反応物 4

HCID 10796Cesium carbonateHCID 312751,4-DioxaneHCID 16217654tert-butyl 4-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole-1-carboxylateHCID 136377183HCID 136377183、化合物

生成物 1

HCID 136377184HCID 136377184、化合物収率 51.3%

試薬・触媒・溶媒 2

HCID 75412134
Dicyclohexyl(2 inverted exclamation mark,4 inverted exclamation mark,6 inverted exclamation mark-Triisopropyl-3,6-Dimethoxy-[1,1 inverted exclamation mark-Biphenyl]-2-Yl)Phosphine-(2-(2-Aminoethyl)Phenyl)Palladium(Ii) Chloride
触媒
HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

To a 10 mL microwave vial, was added (3aR,6aS)-tert-butyl 5-(6-(4-chloro-2-hydroxyphenyl)pyridazin-3-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate (0.182 g, 0.437 mmol), tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole-1-carboxylate (0.385 g, 1.310 mmol), chloro[2-(dicyclohexylphosphino)-3,6-dimethoxy-2′,4′,6′-triisopropyl-1,1′-biphenyl][2-(2-aminoethyl)phenyl]palladium(II) (0.035 g, 0.044 mmol) and Cs2CO3 (0.427 g, 1.310 mmol), followed by adding 1,4-dioxane (2 mL) and water (0.5 mL). The reaction mixture was evacuated and filled with N2 twice then heated at 90° C. overnight. The reaction mixture was filtered through celite and washed with DMSO and MeOH. The filtrate was acidified with 1N HCl and stirred at RT for 3 hour, then extracted with DCM. The aqueous layer was basified with 2M NH2 in MeOH and a brownish precipitate formed, which was filtered and washed with DMSO to afford a grey solid 2-(6-((3aR,6aS)-hexahydropyrrolo[3,4-c]pyrrol-2(1H)-yl)pyridazin-3-yl)-5-(1H-pyrazol-4-yl)phenol (82 mg, 0.224 mmol, 51.2% yield). MS (M+1)=349.1. The DMSO wash solution was concentrated to afford a DMSO solution of desired (3aR,6aS)-tert-butyl 5-(6-(2-hydroxy-4-(1H-pyrazol-4-yl)phenyl)pyridazin-3-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate (75 mg, 0.167 mmol, 38% yield), MS (M+1)=449.1, which was used directly in the next step.

後処理

  1. customThe reaction mixture was evacuated
  2. additionfilled with N2 twice
  3. filtrationThe reaction mixture was filtered through celite
  4. washwashed with DMSO and MeOH
  5. extractionextracted with DCM
  6. customa brownish precipitate formed
  7. filtrationwhich was filtered
  8. washwashed with DMSO

出典と根拠

ORDレコード
ord-9acbf1474aaa4c33b9c0c05ea553976e
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08729263B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート