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Nitrogen → 3-(3-chloro-4-((1-(4-chloro-3-fluorophenyl)-2-methylpropan-2-yl)amino)phenyl)-2,6-dimethylpyrimidin-4(3H)-one

HRID 56310
ノート
印刷プレビュー

反応式

HRID 56310 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]([CH3:21])([CH3:20])[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([F:19])[CH:13]=1.C[Al](C)C.N#N.FC1C=C(C=CC=1)O[CH2:33][C:34]([NH:36]/[C:37](/[CH3:43])=[CH:38]\[C:39](OC)=[O:40])=O>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[C:6]([N:8]2[C:39](=[O:40])[CH:38]=[C:37]([CH3:43])[N:36]=[C:34]2[CH3:33])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]([CH3:21])([CH3:20])[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([F:19])[CH:13]=1
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 4

HCID 947NitrogenHCID 16682925Trimethylaluminum2 回HCID 90022556Methyl 3-(2-(3-fluorophenoxy)acetamido)crotonate2 回HCID 1179660612-chloro-N1-(1-(4-chloro-3-fluorophenyl)-2-methylpropan-2-yl)benzene-1,4-diamine

生成物 1

HCID 900223713-(3-chloro-4-((1-(4-chloro-3-fluorophenyl)-2-methylpropan-2-yl)amino)phenyl)-2,6-dimethylpyrimidin-4(3H)-one
収率 33.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒3 回

実験手順

To a solution of 2-chloro-N1-(1-(4-chloro-3-fluorophenyl)-2-methylpropan-2-yl)benzene-1,4-diamine (408 mg, 1.25 mmol) in toluene (15 mL) was added trimethylaluminium (2.5 mL, 5.00 mmol, 2.0 M in toluene) dropwise under N2 and the mixture was stirred at rt for 30 min after addition was completed. A solution of (Z)-methyl 3-(2-(3-fluorophenoxy)acetamido)but-2-enoate (295 mg, 1.88 mmol) in toluene (5 mL) was added slowly and the resulting mixture was stirred at rt for 22 h. Trimethylaluminium (2.0 mL, 4.00 mmol, 2 M in toluene) was then added dropwise and the mixture was stirred at rt for 30 min. A solution of (Z)-methyl 3-(2-(3-fluorophenoxy)acetamido)but-2-enoate (295 mg, 1.88 mmol) in toluene (3 mL) was added and the mixture was stirred further for 18 h. The mixture was quenched with saturated NH4Cl aqueous solution (50 mL) and filtered and the organic phase was separated from the filtrate. The aqueous phase was extracted with EtOAc (30 mL×3). The combined organic layers were washed with brine (30 mL×2), dried over anhydrous Na2SO4 (15 g) and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=2:3) to give the title compound as a yellow solid (183 mg, 33.7%). The compound was characterized by the following spectroscopic data:

後処理

  1. additionafter addition
  2. stirringthe resulting mixture was stirred at rt for 22 h
  3. stirringthe mixture was stirred at rt for 30 min
  4. stirringthe mixture was stirred further for 18 h
  5. customThe mixture was quenched with saturated NH4Cl aqueous solution (50 mL)
  6. filtrationfiltered
  7. customthe organic phase was separated from the filtrate
  8. extractionThe aqueous phase was extracted with EtOAc (30 mL×3)
  9. washThe combined organic layers were washed with brine (30 mL×2)
  10. dry with materialdried over anhydrous Na2SO4 (15 g)
  11. concentrationconcentrated in vacuo
  12. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=2:3)

出典と根拠

ORDレコード
ord-038ed3ba5fb04478b5c5d615d9c72808
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434695B2

反応ノート

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