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Methanol → HCID 178420310、化合物

HRID 1854492
ノート
印刷プレビュー

反応式

HRID 1854492 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([C:14](=[N:25][NH2:26])[C:15]2[C:20](Cl)=[CH:19][N:18]=[C:17]3[NH:22][CH:23]=[CH:24][C:16]=23)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(C)([O-])C.[Na+].CO>CN1C(=O)CCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(P(C2CCCCC2)C2[C-](CCP(C(C)(C)C)C(C)(C)C)C=CC=2)CCCCC1.[CH-]1C=CC=C1.[Fe+2]>[CH2:1]([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([C:14]2[C:15]3=[C:16]4[CH:24]=[CH:23][NH:22][C:17]4=[N:18][CH:19]=[C:20]3[NH:26][N:25]=2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=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 3

HCID 887MethanolHCID 23676156Sodium t-butoxideHCID 866371884-((1-benzylpiperidin-3-yl)(hydrazono)methyl)-5-chloro-1H-pyrrolo[2,3-b]pyridine

生成物 1

HCID 178420310HCID 178420310、化合物収率 19%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒3 回
HCID 131732182
1-Dicyclohexylphosphino-2-di-t-butylphosphinoethyl ferrocene
触媒
HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
160 °C

実験手順

A mixture of 4-((1-benzylpiperidin-3-yl)(hydrazono)methyl)-5-chloro-1H-pyrrolo[2,3-b]pyridine (1.04 g, 2.84 mmol), sodium tert-butoxide (0.652 g, 6.78 mmol), palladium acetate (0.0064 g, 0.028 mmol) and (R)-1-[(S)-2-(dicyclohexylphosphino)ferrocenyl]ethyl-di-tert-butyl phosphine (0.016 g, 0.028 mmol) in NMP (10 mL) was heated in the microwave at about 160° C. for about 30 min. Additional palladium acetate (0.0064 g, 0.028 mmol) and (R)-1-[(S)-2-(dicyclohexylphosphino)ferrocenyl]ethyl-di-tert-butyl phosphine (0.016 g, 0.028 mmol) were added and the mixture was heated in a microwave at about 160° C. for about 15 min. Additional palladium acetate (0.003 g, 0.014 mmol) and (R)-1-[(−2-(dicyclohexylphosphino)ferrocenyl]ethyl-di-tert-butyl phosphine (0.008 g, 0.014 mmol) were added and the mixture was again heated at about 160° C. for about 8 min. The solvent was removed under reduced pressure and the residue was partitioned between water (25 mL) and EtOAc (25 mL). The organic phase was washed with brine (20 mL), dried over anhydrous MgSO4, decolorized with charcoal and filtered. The solvent was removed under reduced pressure and the residue purified by silica gel chromatography, eluting first with DCM (1 L), a mixture of 98:1:1 DCM:TEA:MeOH (1 L) and then with a mixture of 97:1:2 DCM:TEA:MeOH (1 L) to yield 1-(1-benzylpiperidin-3-yl)-3,6-dihydropyrazolo[4,3-d]pyrrolo[2,3-b]pyridine (0.18 g, 0.54 mmol, 19%) as a brown solid: LC/MS (Table 2, Method a) Rt=1.36 min; MS m/z: 332 (M+H)+.

後処理

  1. temperaturethe mixture was heated in a microwave at about 160° C. for about 15 min
  2. temperaturethe mixture was again heated at about 160° C. for about 8 min
  3. customThe solvent was removed under reduced pressure
  4. customthe residue was partitioned between water (25 mL) and EtOAc (25 mL)
  5. washThe organic phase was washed with brine (20 mL)
  6. dry with materialdried over anhydrous MgSO4
  7. filtrationfiltered
  8. customThe solvent was removed under reduced pressure
  9. customthe residue purified by silica gel chromatography
  10. washeluting first with DCM (1 L)
  11. additiona mixture of 98:1:1 DCM
  12. additionTEA:MeOH (1 L) and then with a mixture of 97:1:2 DCM

出典と根拠

ORDレコード
ord-88667919e3e64b92bda8c7527d000a4b
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08962629B2

反応ノート

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