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Hydrochloric Acid → 6-(2-Hydroxypropan-2-yl)-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide

HRID 629109
ノート
印刷プレビュー

反応式

HRID 629109 の反応式
Cl[C:2]1[C:21]([C:22]2[CH:23]=[N:24][CH:25]=[N:26][CH:27]=2)=[CH:20][C:5]([C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][C:16]([F:19])([F:18])[F:17])=[CH:11][CH:10]=2)=[O:7])=[CH:4][N:3]=1.C([Sn](CCCC)(CCCC)C(OCC)=C)CCC.C([O:48][C:49]([C:51]1C(C2C=NC=NC=2)=CC(C(NC2C=CC(OC(F)(F)F)=CC=2)=O)=CN=1)=[CH2:50])C.Cl.C([O-])([O-])=O.[Na+].[Na+].C(C1C(C2C=NC=NC=2)=CC(C(NC2C=CC(OC(F)(F)F)=CC=2)=O)=CN=1)(=O)C.C[Mg+].[Br-].C1COCC1.C1(C)C=CC=CC=1.[NH4+].[Cl-]>C(Cl)Cl.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.O1CCOCC1>[OH:48][C:49]([C:2]1[C:21]([C:22]2[CH:23]=[N:24][CH:25]=[N:26][CH:27]=2)=[CH:20][C:5]([C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][C:16]([F:19])([F:18])[F:17])=[CH:11][CH:10]=2)=[O:7])=[CH:4][N:3]=1)([CH3:51])[CH3:50]
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

13

反応物 9

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 25517Ammonium ChlorideHCID 619414Stannane, tributyl(1-ethoxyethenyl)-HCID 22635083Tetrahydrofuran tolueneHCID 722034246-Chloro-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide
HCID 89906819
6-acetyl-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide
HCID 899077966-(1-ethoxyvinyl)-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide
HCID 178418689HCID 178418689、化合物

生成物 1

HCID 899080026-(2-Hydroxypropan-2-yl)-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
110 °C

実験手順

6-Chloro-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide (Example 56, 100 mg, 0.253 mmol), tributyl(1-ethoxyvinyl)stannane (0.103 mL, 0.304 mmol), Pd(Ph3P)4 (29.3 mg, 0.025 mmol) and dioxane (1 mL) were added to a vial, which was sealed, evacuated/purged with argon and the RM was stirred at 110° C. for 2 h. The solvent was evaporated off under reduced the crude 6-(1-ethoxyvinyl)-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide (100 mg, 0.232 mmol) was treated with 4 M HCl in dioxane (2 mL, 8.00 mmol), stirred at RT for 2 h and then treated with excess aq. Na2CO3 and the solvent was evaporated off under reduced pressure to give a residue which was purified by flash chromatography (RediSep® Silica gel column, 24 g, EtOAc/n-hexane from 50% to 70% EtOAc). The 6-acetyl-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide (25 mg, 0.062 mmol) was dissolved in DCM (3 mL), cooled to −60° C. and treated dropwise with a solution of MeMgBr 1.4 M in THF/toluene (1:3) (0.089 mL, 0.124 mmol) at The RM was stirred for 1.5 h at −60° C., then treated with a sat. aq. NH4Cl solution and extracted with DCM. The combined extracts were dried over MgSO4 and the solvent was evaporated off under reduced pressure to give the crude product which was purified by preparative SFC (Column NH2; gradient 12% to 17% in 6 min.) and lyophilized in water/MeCN to afford the title compound. UPLC-MS (Condition 2) tR 0.79-0.94 min, m/z=419.1 [M+H]+; 1H-NMR (600 MHz, DMSO-d6) δ ppm 1.49 (s, 6H) 5.02 (br. s, 1H) 7.39 (d, J=8.40 Hz, 2H) 7.87 (d, J=9.10 Hz, 2H) 8.11 (d, J=2.19 Hz, 1H) 8.77 (s, 2H) 9.09 (d, J=2.20 Hz, 1H) 9.13 (s, 1H) 10.55 (s, 1H).

後処理

  1. customwas sealed
  2. customevacuated/purged with argon
  3. customThe solvent was evaporated off
  4. stirringstirred at RT for 2 h
  5. customthe solvent was evaporated off under reduced pressure
  6. customto give a residue which
  7. customwas purified by flash chromatography (RediSep® Silica gel column, 24 g, EtOAc/n-hexane from 50% to 70% EtOAc)
  8. temperaturecooled to −60° C.
  9. stirringwas stirred for 1.5 h at −60° C.
  10. extractionextracted with DCM
  11. dry with materialThe combined extracts were dried over MgSO4
  12. customthe solvent was evaporated off under reduced pressure
  13. customto give the crude product which
  14. customwas purified by preparative SFC (Column NH2; gradient 12% to 17% in 6 min.)

出典と根拠

ORDレコード
ord-21662d908c964c0cb86d4180e9329072
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09315489B2

反応ノート

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