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Cesium fluoride → Methyl 2-chloro-4-methyl-6-(3-methyl-1-tosyl-1H-indol-4-yl)nicotinate

HRID 80819
ノート
印刷プレビュー

反応式

HRID 80819 の反応式
[Cl:1][C:2]1[N:11]=[C:10](Cl)[CH:9]=[C:8]([CH3:13])[C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH3:14][C:15]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][C:22]=2B2OC(C)(C)C(C)(C)O2)[N:17]([S:33]([C:36]2[CH:42]=[CH:41][C:39]([CH3:40])=[CH:38][CH:37]=2)(=[O:35])=[O:34])[CH:16]=1.[F-].[Cs+]>CN(C=O)C.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>[Cl:1][C:2]1[N:11]=[C:10]([C:22]2[CH:21]=[CH:20][CH:19]=[C:18]3[C:23]=2[C:15]([CH3:14])=[CH:16][N:17]3[S:33]([C:36]2[CH:42]=[CH:41][C:39]([CH3:40])=[CH:38][CH:37]=2)(=[O:35])=[O:34])[CH:9]=[C:8]([CH3:13])[C:3]=1[C:4]([O:6][CH3:7])=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 25953Cesium fluorideHCID 46911843Methyl 2,6-dichloro-4-methylnicotinateHCID 712404273-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1-tosyl-1H-indole

生成物 1

HCID 86690266Methyl 2-chloro-4-methyl-6-(3-methyl-1-tosyl-1H-indol-4-yl)nicotinate

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 6228Dimethylformamide溶媒

実験手順

A mixture of methyl 2,6-dichloro-4-methylnicotinate (0.250 g, 1.14 mmol), 3-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1-tosyl-1H-indole (Example 6) (0.514 g, 1.25 mmol), Pd(Ph3P)4 (0.131 g, 0.114 mmol), and CsF (0.345 g, 2.27 mmol), in DMF (5 mL) was heated at 110° C. for 6 h. At that time the vessel was removed from the oil bath and allowed to cool to rt. The mixture was diluted with brine (50 mL) and EtOAc (50 mL). The layers were mixed and then separated. The aqueous layer was further extracted with EtOAc (50 mL) and the combined organic layers were dried (Na2SO4), filtered, and concentrated. The residue was then purified via FCC (0-10% EtOAc/heptane) to give the title compound. MS ESI m/z 469.0 & 470.9 (M+H)+.

後処理

  1. customAt that time the vessel was removed from the oil bath
  2. additionThe mixture was diluted with brine (50 mL) and EtOAc (50 mL)
  3. additionThe layers were mixed
  4. customseparated
  5. extractionThe aqueous layer was further extracted with EtOAc (50 mL)
  6. dry with materialthe combined organic layers were dried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was then purified via FCC (0-10% EtOAc/heptane)

出典と根拠

ORDレコード
ord-ebf578b16e9146c59bf97ba1928ff07a
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846656B2

反応ノート

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