Hydrochloric Acid → HCID 178444959、化合物

HRID 1609289

反応式

HRID 1609289 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 178444959HCID 178444959、化合物収率 62.1%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3e963d16433042aeab9b5a885ea80189
出典データセット
uspto-grants-1995_03
特許番号
US05399703

関連ノート

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