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Binap, (A+-)- → Morpholin-4-yl(5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}biphenyl-3-yl)methanone

HRID 530388
ノート
印刷プレビュー

反応式

HRID 530388 の反応式
Cl[C:2]1[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][N:3]=1.[NH2:12][C:13]1[CH:14]=[C:15]([C:25]([N:27]2[CH2:32][CH2:31][O:30][CH2:29][CH2:28]2)=[O:26])[CH:16]=[C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:18]=1.CC(C)([O-])C.[Na+].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1>C1(C)C=CC=CC=1.C(OCC)(=O)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[N:27]1([C:25]([C:15]2[CH:16]=[C:17]([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)[CH:18]=[C:13]([NH:12][C:2]3[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][N:3]=3)[CH:14]=2)=[O:26])[CH2:28][CH2:29][O:30][CH2:31][CH2:32]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 634876Binap, (A+-)-HCID 27739122-Chloro-4-(trifluoromethyl)pyrimidineHCID 23676156Sodium t-butoxideHCID 90041595(5-Aminobiphenyl-3-yl)(morpholin-4-yl)methanone

生成物 1

HCID 90041497Morpholin-4-yl(5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}biphenyl-3-yl)methanone

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 1140Toluene溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 2-chloro-4-(trifluoromethyl)pyrimidine (34 mg, 0.186 mmol), (5-aminobiphenyl-3-yl)(morpholin-4-yl)methanone (63.1 mg, 0.224 mmol), sodium tert-butoxide, Pd2(dba)3 (9.64 mg, 0.009 mmol) and BINAP (11.6 mg, 0.019 mmol) in toluene (0.931 mL) was heated to 130° C. in a microwave reactor for 30 minutes, then allowed to cool to room temperature. The reaction mixture was diluted with ethyl acetate (30 mL) and was washed with 0.1 M HCl (30 mL) followed by brine (30 mL). The aqueous phases were further extracted with ethyl acetate (30 mL), then the combined organic extracts were dried over sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by silica gel column chromatography (ethyl acetate/hexanes) provided morpholin-4-yl(5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}biphenyl-3-yl)methanone as a white solid. MS ESI calc'd. for C22H20F3N4O2 [M+H]+ 429, found 429. 1H NMR (400 MHz, CDCl3): δ 8.69 (d, J=4.9 Hz, 1H); 7.92 (s, 1H); 7.80 (s, 1H); 7.71 (s, 1H); 7.63 (d, J=7.6 Hz, 2H); 7.48 (t, J=7.5 Hz, 2H); 7.40 (d, J=6.8 Hz, 2H); 7.15-7.03 (m, 1H); 3.97-3.44 (m, 8H).

後処理

  1. washwas washed with 0.1 M HCl (30 mL)
  2. extractionThe aqueous phases were further extracted with ethyl acetate (30 mL)
  3. dry with materialthe combined organic extracts were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-06e36aa148a946778a428246119595ed
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09353066B2

反応ノート

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