4-Nitrobenzyl alcohol → HCID 20140840、化合物

HRID 1252217

反応式

HRID 1252217 の反応式
[C:1]([C:4]([CH3:21])([CH3:20])[CH2:5][CH2:6][C:7]([O:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][CH:12]=1)=[O:8])([OH:3])=[O:2].CC1(C)CCC(=O)OC1=O.[N+](C1C=CC(CO)=CC=1)([O-])=O.[CH3:43][O:44][C:45]1[CH:52]=[CH:51][C:48]([CH2:49]Cl)=[CH:47][CH:46]=1>CN(C)C=O.O.C(N(CC)CC)C>[CH3:43][O:44][C:45]1[CH:52]=[CH:51][C:48]([CH2:49][O:2][C:1]([C:4]([CH3:21])([CH3:20])[CH2:5][CH2:6][C:7]([O:9][CH2:10][C:11]2[CH:12]=[CH:13][C:14]([N+:17]([O-:19])=[O:18])=[CH:15][CH:16]=2)=[O:8])=[O:3])=[CH:47][CH:46]=1

参加物

8

反応物 4

HCID 692754-Nitrobenzyl alcoholHCID 699934-Methyloxybenzyl chlorideHCID 76247Dihydro-3,3-dimethyl-2H-pyran-2,6(3H)-dioneHCID 20140795p-Nitrobenzyl 4-carboxy-4-methylvalerate

生成物 1

HCID 20140840HCID 20140840、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒

反応条件

温度
80 °C

実験手順

To a solution of p-nitrobenzyl 4-carboxy-4-methylvalerate (17.26 g) in dry dimethylformamide (100 ml), prepared by the procedure similar to that described in Example 174 from 2,2-dimethylglutaric anhydride and p-nitrobenzyl alcohol, was added p-methoxybenzyl chloride (9.16 g) and triethylamine (5.91 g). The reaction mixture was stirred at 80° C. for 9.5 hours, diluted with water and extracted with diethyl ether. The extract was washed successively with aqueous potassium carbonate, water, dilute hydrochloric acid and again water, dried over anhydrous sodium sulfate and evaporated to give p-nitrobenzyl 4-p-methoxybenzyloxycarbonyl-4-methylvalerate.

後処理

  1. extractionextracted with diethyl ether
  2. washThe extract was washed successively with aqueous potassium carbonate, water, dilute hydrochloric acid and again water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-2bae3c7b3497440ab93648332a424e42
出典データセット
uspto-grants-1988_05
特許番号
US04742052

関連ノート

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