Hydrochloric Acid → HCID 178444959, 화합물

HRID 1609289

반응식

HRID 1609289 반응식
[NH:1]1[C:5]([CH:6]([O:8][C:9]2[CH:10]=[C:11]([CH:20]=[CH:21][CH:22]=2)[O:12][C:13]2[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=2[NH2:15])[CH3:7])=[N:4][N:3]=[N:2]1.C(N(CC)CC)C.[CH2:30]([O:36][C:37]1[CH:45]=[CH:44][C:40]([C:41](Cl)=[O:42])=[CH:39][CH:38]=1)[CH2:31][CH2:32][CH2:33][CH2:34][CH3:35].Cl>C(Cl)Cl.C1C=CC=CC=1>[NH:4]1[C:5]([CH:6]([O:8][C:9]2[CH:10]=[C:11]([CH:20]=[CH:21][CH:22]=2)[O:12][C:13]2[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=2[NH:15][C:41](=[O:42])[C:40]2[CH:39]=[CH:38][C:37]([O:36][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])=[CH:45][CH:44]=2)[CH3:7])=[N:1][N:2]=[N:3]1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 170235Benzoyl chloride, 4-(hexyloxy)-HCID 178466631HCID 178466631, 화합물

생성물 1

HCID 178444959HCID 178444959, 화합물수율 62.1%

시약·촉매·용매 2

HCID 241Benzene용매HCID 6344Dichloromethane용매

실험 절차

In 30 ml of methylene chloride were dissolved 2.1 g of 2-[3-[1-(1H-tetrazol-5-yl)ethoxy]phenoxy]aniline and 2.2 g of triethylamine, followed by dropwise addition of a solution of 1.7 g of 4-hexyloxybenzoyl chloride in benzene with ice-cooling and stirring. The mixture was stirred at room temperature overnight and refluxed for 1 hour. To the reaction mixture was added ice-water and after the mixture was acidified with diluted hydrochloric acid, the methylene chloride layer was separated. The methylene chloride solution was dried over magnesium sulfate and concentrated and the oily residue was subjected to silica gel column chromatography using chloroform-methanol (100:1) as the eluent to give 2.2 g of the title compound as a light yellow oil.

후처리

  1. temperaturecooling
  2. stirringThe mixture was stirred at room temperature overnight
  3. temperaturerefluxed for 1 hour
  4. customthe methylene chloride layer was separated
  5. dry with materialThe methylene chloride solution was dried over magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3e963d16433042aeab9b5a885ea80189
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05399703

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