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Chloroform → N-methoxy-N-methyl-4-nitro-2'-methoxymethoxy-6'-methoxy-biphenyl-2-carboxamide

HRID 1358113
ノート
印刷プレビュー

反応式

HRID 1358113 の反応式
C([Li])CCC.[CH3:6][O:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH2:15][O:16][CH3:17])[CH:9]=1.[CH3:18][O:19][N:20]([CH3:33])[C:21](=[O:32])[C:22]1[CH:27]=[C:26]([N+:28]([O-:30])=[O:29])[CH:25]=[CH:24][C:23]=1Br.C(Cl)(Cl)Cl>C1COCC1.[Cl-].[Zn+2].[Cl-].[Pd](Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[CH3:18][O:19][N:20]([CH3:33])[C:21]([C:22]1[C:23]([C:9]2[C:8]([O:7][CH3:6])=[CH:13][CH:12]=[CH:11][C:10]=2[O:14][CH2:15][O:16][CH3:17])=[CH:24][CH:25]=[C:26]([N+:28]([O-:30])=[O:29])[CH:27]=1)=[O:32]
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 6212ChloroformHCID 5426211-Methoxy-3-(methoxymethoxy)benzeneHCID 18188772N-methoxy-N-methyl-2-bromo-5-nitrobenzamideHCID 178418339Butyllithium

生成物 1

HCID 18189308N-methoxy-N-methyl-4-nitro-2'-methoxymethoxy-6'-methoxy-biphenyl-2-carboxamide収率 88%

試薬・触媒・溶媒 3

HCID 3007855
Zincchloride
触媒
HCID 6102075Dichlorobis(triphenylphosphine)palladium触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Butyllithium (8.28 ml. of 2.5M in hexane, 20.69 mmole) was added to a solution of 1-methoxy-3 methoxymethoxy benzene (3.62 g., 21.55 mmole, (T. Kaufman, R. Srivastava, R. Sindelar, J. Med. Chem. 1995, 38, 1437-1445) in. THF (15 mL) at −30° C. The solution was stirred at ambient temperature for 1 hour, cooled to at 0° C. and anhydrous zinc chloride beads (3.5 g, 25.67 mmole) added. The mixture was stirred for 2 hours at 25°. Then a solution of N-methoxy-N-methyl-2-bromo-5-nitrobenzamide (5.00 g, 17.24 mmole) dissolved in THF (20 mL) was added. Bis (triphenylphosphine) palladium dichloride (600 mg.) was added and the solution was stirred at 65° C. for 15 hours. After cooling, chloroform was added and the solution stirred with aqueous KHCO3. The precipitated zinc salts were filtered, the water layer removed and the organic layer dried (Na2SO4), filtered concentrated under reduced pressure and the residuepurified on silica gel eluting with 8% ethyl acetate in CH2Cl2 to provide the titled compound (5.68 g, 88% yield).

後処理

  1. customat −30° C
  2. additionadded
  3. stirringThe mixture was stirred for 2 hours at 25°
  4. additionwas added
  5. stirringthe solution was stirred at 65° C. for 15 hours
  6. temperatureAfter cooling
  7. filtrationThe precipitated zinc salts were filtered
  8. customthe water layer removed
  9. dry with materialthe organic layer dried (Na2SO4)
  10. filtrationfiltered
  11. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-648bf1047d70405d923fd46975cfcfba
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06593480B2

反応ノート

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