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7-Chlorothieno[3,2-b]pyridine → HCID 66599084、化合物

HRID 1047450
ノート
印刷プレビュー

反応式

HRID 1047450 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6]N=[C:4]2[CH:8]=[CH:9][S:10][C:3]=12.[Li][CH2:12]CCC.Br[C:17]1[N:22]=[CH:21][C:20]([CH2:23][N:24]([CH2:32][CH2:33][O:34][CH3:35])C(=O)OC(C)(C)C)=[CH:19][CH:18]=1>C1COCC1.[Cl-].[Cl-].[Zn+2].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[C:3]2[S:10][C:9]([C:17]3[N:22]=[CH:21][C:20]([CH2:23][NH:24][CH2:32][CH2:33][O:34][CH3:35])=[CH:19][CH:18]=3)=[CH:8][C:4]=2[CH:12]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 112752517-Chlorothieno[3,2-b]pyridineHCID 57919609tert-Butyl [(6-Bromopyridin-3-yl)methyl](2-methoxyethyl)carbamateHCID 178418339Butyllithium

生成物 1

HCID 66599084HCID 66599084、化合物収率 83.1%

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 7-chlorothieno[3,2-b]pyridine 6 (7.37 g, 43.4 mmol, 1.5 eq) in THF (70 mL) at −10° C. in a 250 mL round-bottom flask was added n-BuLi (17.38 mL, 43.4 mmol, 1.5 eq). After 1 h, ZnCl2 (1M in ether) (43.4 mL, 43.4 mmol, 1.5 eq) was added at −10° C. and the reaction mixture was allowed to warm up to r.t. After 1 h, Pd(PPh3)4 (0.669 g, 0.579 mmol, 0.02 eq) and bromide 10 (10 g, 29 mmol, 1 eq) in THF (10.5 mL) were added and the mixture was heated to reflux for 1 h. After cooling to room temperature the reaction mixture was concentrated to dryness. DCM (200 mL)/water (160 mL)/NH4OH (40 mL) were added to the solid and the resultant mixture (an emulsion) was stirred for 1 h. Brine (50 ml) was added to the emulsion and the stirring was continued for an additional 10 min. The mixture was then filtered through a paper filter and phases were separated. The aqueous phase was extracted with DCM (2×50 mL). The organic phases were combined, dried over Na2SO4 and concentrated to dryness. MTBE (30 mL) was added to the solid and the suspension was stirred for 30 min. The solid was collected by filtration, washed with MTBE (2×5 mL) and dried to afford of 11 as a beige solid (8.02 g, 64% yield). MS (m/z): 434.2 (M+1).

後処理

  1. waitAfter 1 h
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 1 h
  4. temperatureAfter cooling to room temperature the reaction mixture
  5. concentrationwas concentrated to dryness
  6. additionDCM (200 mL)/water (160 mL)/NH4OH (40 mL) were added to the solid
  7. additionBrine (50 ml) was added to the emulsion
  8. waitthe stirring was continued for an additional 10 min
  9. filtrationThe mixture was then filtered through a paper
  10. filtrationfilter
  11. customphases were separated
  12. extractionThe aqueous phase was extracted with DCM (2×50 mL)
  13. dry with materialdried over Na2SO4
  14. concentrationconcentrated to dryness
  15. additionMTBE (30 mL) was added to the solid
  16. stirringthe suspension was stirred for 30 min
  17. filtrationThe solid was collected by filtration
  18. washwashed with MTBE (2×5 mL)
  19. customdried

出典と根拠

ORDレコード
ord-bfc483023fc94429b71c718f62e39516
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569503B2

反応ノート

読み込み中…

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