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Toluene → Ethyl 2-(4-methoxybenzoyl)-4-nitromethyl-3-(1,3-benzodioxole-5-yl)butyrate

HRID 54570
ノート
印刷プレビュー

反応式

HRID 54570 の反応式
[CH3:1][O:2][C:3]1[CH:16]=[CH:15][C:6]([C:7]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[O:8])=[CH:5][CH:4]=1.[N+:17]([CH:20]=[CH:21][C:22]1[CH:30]=[CH:29][C:25]2OCOC=2C=1)([O-:19])=[O:18].[C:31]([O:34][CH2:35][CH3:36])(=[O:33])C.[C:37]1(C)C=CC=CC=1>C(Cl)Cl.N12CCCN=C1CCCCC2>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([CH:9]([CH:22]([C:30]2[CH:29]=[CH:25][C:36]3[O:33][CH2:31][O:34][C:35]=3[CH:37]=2)[CH2:21][CH2:20][N+:17]([O-:19])=[O:18])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[O:8])=[CH:15][CH:16]=1
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

7

反応物 4

HCID 1140Toluene2 回HCID 8857Ethyl AcetateHCID 76150Benzenepropanoic acid, 4-methoxy-beta-oxo-, ethyl esterHCID 949455-(2-Nitroethenyl)-1,3-benzodioxole

生成物 1

HCID 22322609Ethyl 2-(4-methoxybenzoyl)-4-nitromethyl-3-(1,3-benzodioxole-5-yl)butyrate

試薬・触媒・溶媒 2

HCID 81184
1,8-Diazabicyclo(5.4.0)undec-7-ene
触媒
2 回
HCID 6344Dichloromethane溶媒

反応条件

温度
80 °C

実験手順

To ethyl (4-methoxybenzoyl)acetate (23.0 g, 0.104 mol), prepared by the method of Krapcho et al., Org. Syn. 47, 20 (1967), and 5-(2-nitrovinyl)-1,3-benzodioxole (17.0 g, 0.088 mol) dissolved in 180 mL of toluene and heated to 80° C. was added 1,8-diazabicyclo[5,4,0]undec-7-ene (DBU, 0.65 g) with stirring. The mixture was heated until all the nitro starting material dissolved. The solution was stirred without heating for 30 minutes and then an additional 0.65 g of DBU was added. After stirring an additional 45 minutes, thin layer chromatography (5% ethyl acetate in methylene chloride) indicated the absence of nitro starting material. Toluene (200 mL) was added, and the organic phase was washed with dilute hydrochloric acid and NaCl solution. The organic phase was dried over sodium sulfate and then concentrated under reduced pressure. The residue obtained was chromatographed on silica gel eluting with 3:1 hexane-ethyl acetate to give 21.22 g of the desired product as a mixture of isomers and 9.98 g. of recovered ethyl (4-methoxybenzoyl)acetate.

後処理

  1. dissolutiondissolved
  2. stirringThe solution was stirred
  3. temperaturewithout heating for 30 minutes
  4. stirringAfter stirring an additional 45 minutes
  5. washthe organic phase was washed with dilute hydrochloric acid and NaCl solution
  6. dry with materialThe organic phase was dried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue obtained
  9. customwas chromatographed on silica gel eluting with 3:1 hexane-ethyl acetate

出典と根拠

ORDレコード
ord-19a1f02e2a9c4cf59ae0b3f37bc6aeab
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05622971

反応ノート

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