ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Cesium carbonate → tert-Butyl 5-[1-(2,2-dimethylpropyl)-3-methyl-2-oxo-2,3-dihydro-1H-imidazo-[4,5-b]pyridin-5-yl]-3,3a,4,6a-tetrahydrocyclopenta[c]pyrrole-2(1H)-carboxylate

HRID 629872
ノート
印刷プレビュー

反応式

HRID 629872 の反応式
FC(F)(F)S(O[C:7]1[CH2:8][CH:9]2[CH2:13][N:12]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:11][CH:10]2[CH:21]=1)(=O)=O.[C:24]([O-])(=O)C.[K+].Cl[C:30]1[N:35]=[C:34]2[N:36]([CH3:44])[C:37](=[O:43])[N:38]([CH2:39][CH:40]3[CH2:42][CH2:41]3)[C:33]2=[CH:32][CH:31]=1.C([O-])([O-])=O.[Cs+].[Cs+]>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C.O.O1CCOCC1>[CH3:24][C:40]([CH3:41])([CH3:42])[CH2:39][N:38]1[C:33]2[C:34](=[N:35][C:30]([C:7]3[CH2:8][CH:9]4[CH2:13][N:12]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:11][CH:10]4[CH:21]=3)=[CH:31][CH:32]=2)[N:36]([CH3:44])[C:37]1=[O:43]
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

9

反応物 4

HCID 10796Cesium carbonateHCID 517044Potassium AcetateHCID 772308275-chloro-1-(cyclopropylmethyl)-3-methyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-oneHCID 89303915tert-butyl 5-(((trifluoromethyl)sulfonyl)oxy)-3,3a,6,6a-tetrahydrocyclopenta[c]pyrrole-2(1H)-carboxylate

生成物 1

HCID 71136709
tert-Butyl 5-[1-(2,2-dimethylpropyl)-3-methyl-2-oxo-2,3-dihydro-1H-imidazo-[4,5-b]pyridin-5-yl]-3,3a,4,6a-tetrahydrocyclopenta[c]pyrrole-2(1H)-carboxylate

試薬・触媒・溶媒 4

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒HCID 178418851HCID 178418851、化合物触媒HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

tert-Butyl 5-{[(trifluoromethyl)sulfonyl]oxy}-3,3a,4,6a-tetrahydrocyclopenta-[c]pyrrole-2(1H)-carboxylate (8-2, 2 g, 5.5 mmol, 1.0 equiv), bis(pinocolato)diboron (1.5 g, 6.1 mmol, 1.1 equiv), potassium acetate (1.6 g, 16.8 mmol, 3.0 equiv) and PdCl2(dppf) (0.288 g, 0.392 mmol, 0.07 equiv) were added to anhydrous 1,4-dioxane (7 mL) and heated to 60° C. After 18 h, the reaction contents were cooled to RT, followed by the subsequent addition of water (1.4 mL), 5-chloro-1-(2,2-dimethylpropyl)-3-methyl-1,3-dihydro-2H-imidazo[4,5-b]-pyridin-2-one (1-4, 1.4 g, 5.5 mmol, 1.0 equiv), Cs2CO3 (3.6 g, 11.1 mmol, 2.00 equiv) and Bis(tri-tert-butylphosphine)palladium(0) (0.372 g, 0.728 mmol, 0.13 equiv). The resulting mixture was heated to 60° C. for 4.5 h. Following this duration, LCMS showed consumption of starting material. The contents were then cooled to room temperature, diluted with ethyl acetate (50 mL), filtered through Celite and rinsed with ethyl acetate (3×50 mL) and water (1×30 mL). The filtrate layers were separated and the combined organics were washed with saturated NaHCO3 (100 mL). The combined aqueous layers were then back-extracted with ethyl acetate (2×50 mL). The combined organics were dried over Na2SO4, filtered and concentrated in vacuo to give a dark red oil. Purification by normal-phase chromatography (0-50% EtOAc:Hex) afforded 8-3 as an off-white solid. MS m/z (M+H): calculated=427.55; observed=427.2.

後処理

  1. customthe reaction contents
  2. temperaturewere cooled to RT
  3. temperatureThe resulting mixture was heated to 60° C. for 4.5 h
  4. customconsumption of starting material
  5. temperatureThe contents were then cooled to room temperature
  6. additiondiluted with ethyl acetate (50 mL)
  7. filtrationfiltered through Celite
  8. washrinsed with ethyl acetate (3×50 mL) and water (1×30 mL)
  9. customThe filtrate layers were separated
  10. washthe combined organics were washed with saturated NaHCO3 (100 mL)
  11. extractionThe combined aqueous layers were then back-extracted with ethyl acetate (2×50 mL)
  12. dry with materialThe combined organics were dried over Na2SO4
  13. filtrationfiltered
  14. concentrationconcentrated in vacuo
  15. customto give a dark red oil
  16. customPurification by normal-phase chromatography (0-50% EtOAc:Hex)

出典と根拠

ORDレコード
ord-50801646401448829841a6517ee649a7
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09315518B2

反応ノート

読み込み中…

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