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3-Methoxyaniline → HCID 57825031、化合物

HRID 1668762
ノート
印刷プレビュー

反応式

HRID 1668762 の反応式
Br[C:2]1[CH:3]=[C:4]([C:8]2([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH3:22])=[C:16]([CH3:23])[CH:15]=3)[CH2:12][O:11][C:10]([NH2:13])=[N:9]2)[CH:5]=[CH:6][CH:7]=1.CC(C)([O-])C.[Na+].C(P(C(C)(C)C)C1C=CC=CC=1C1C(CCC)=CC(CCC)=CC=1CCC)(C)(C)C.[CH3:60][O:61][C:62]1[CH:63]=[C:64]([CH:66]=[CH:67][CH:68]=1)[NH2:65]>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].C(OC(=O)C)C.O.C1(C)C=CC=CC=1>[CH2:21]([O:20][C:17]1[CH:18]=[CH:19][C:14]([C:8]2([C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([NH:65][C:64]4[CH:66]=[CH:67][CH:68]=[C:62]([O:61][CH3:60])[CH:63]=4)[CH:3]=3)[CH2:12][O:11][C:10]([NH2:13])=[N:9]2)=[CH:15][C:16]=1[CH3:23])[CH3:22]
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

9

反応物 4

HCID 108243-MethoxyanilineHCID 23676156Sodium t-butoxideHCID 57825006HCID 57825006、化合物HCID 67346612HCID 67346612、化合物

生成物 1

HCID 57825031HCID 57825031、化合物

試薬・触媒・溶媒 4

HCID 9811564Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

A microwave tube was charged with 4-(3-bromo-phenyl)-4-(4-ethoxy-3-methyl-phenyl)-4,5-dihydro-oxazol-2-ylamine (Building Block M, 175 mg, 0.467 mmol, 1.0 eq), sodium tert-butoxide (89 mg, 0.933 mmol, 2.0 eq.), 2-di-t-butylphosphino-2′,4′,6′-tri-1-propyl-1,1′biphenyl (18 mg, 0.042 mmol, 0.042 eq.), tris(dibenzylideneacetone)dipalladium (10 mg, 0.012 mmol, 0.025 eq.) and 3-methoxyaniline (115 mg, 0.933 mmol, 2.0 eq.). After three vacuum-nitrogen cycles, toluene was introduced (1 mL), the tube was scaled and stirred at 100° C. for 16 hours. After cooling to room temperature, water (1 mL) and ethylacetate (1 mL) were added. The organic fraction of the reaction mixture was placed on an SCX column. This was then washed with dichloromethane/methanol. The desired product was obtained by eluting with 2 M ammonia in methanol. Fractions containing the compound were combined and the product purified further using preparative HPLC to yield 95 mg (30% yield) of the title compound as a white solid.

後処理

  1. temperatureAfter cooling to room temperature
  2. washThis was then washed with dichloromethane/methanol

出典と根拠

ORDレコード
ord-879def032ed348c681e98cd211836cab
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07989449B2

反応ノート

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