4-Nitrobenzyl alcohol → HCID 20140840, 화합물

HRID 1252217

반응식

HRID 1252217 반응식
[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

참가 물질

8

반응물 4

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

생성물 1

HCID 20140840HCID 20140840, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2bae3c7b3497440ab93648332a424e42
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04742052

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