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Triethylamine hydrochloride → HCID 178440084、化合物

HRID 1637363
ノート
印刷プレビュー

反応式

HRID 1637363 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:14]=[CH:13][C:12]([CH2:15][N:16]2[C:20]([C:21]([OH:23])=[O:22])=[C:19]([C:24]([OH:27])([CH3:26])[CH3:25])[N:18]=[C:17]2[CH2:28][CH2:29][CH3:30])=[CH:11][CH:10]=1)#[N:2].[N-:31]=[N+:32]=[N-:33].[Na+].Cl.C(N(CC)CC)C.[OH-].[Na+]>O.C1(C)C=CC=CC=1>[OH:27][C:24]([C:19]1[N:18]=[C:17]([CH2:28][CH2:29][CH3:30])[N:16]([CH2:15][C:12]2[CH:11]=[CH:10][C:9]([C:4]3[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=3[C:1]3[NH:33][N:32]=[N:31][N:2]=3)=[CH:14][CH:13]=2)[C:20]=1[C:21]([OH:23])=[O:22])([CH3:25])[CH3:26]
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 11130Triethylamine hydrochlorideHCID 14798Sodium HydroxideHCID 33557Sodium AzideHCID 193491411-(2'-Cyanobiphenyl-4-yl)methyl-4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylic acid

生成物 1

HCID 178440084HCID 178440084、化合物収率 72.4%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 1140Toluene溶媒

反応条件

温度
97.5 °C

実験手順

Into a 500-ml flask equipped with a reflux condenser, thermometer and stirrer were placed 43.5 g (0.10 mole) of ethyl ester of 1-(2'-cyanobiphenyl-4-yl)methyl-4-(1-hydroxy-1-methylethyl) -2-propylimidazole-5-carboxylic acid, 19.5 g (0.30 mole) of sodium azide, 41.3 g (0.30 mole) of triethylamine hydrochloride and 206 ml of toluene. The mixture was heated with stirring to a temperature of 95 to 100° C. to undergo a reaction for 24 hours. After completion of the reaction, the reaction mixture was cooled to room temperature. Then, 35.0 g (0.42 mole) of a 48 wt % aqueous solution of NaOH and 335 ml of water were added. The mixture was fractionated after 2 hours' stirring at room temperature. The aqueous layer was washed and fractionated with the addition of 103 ml of toluene. The aqueous layer was adjusted to a pH of 2 to 3.5 with 36 wt % hydrochloric acid to separate out crystals, which were collected by filtration and dried. The crystals were heated, washed with methanol with stirring, cooled, filtered for collection and dried, giving 32.6 g (0.07 mole) of 4-(1-hydroxy-1-methylethyl) -2-propyl-1-{4-[2-(tetrazole-5-yl)phenyl]phenyl}methylimidazole-5-carboxylic acid (yield 72.4% based on ethyl ester of 1-(2'-cyanobiphenyl-4-yl)methyl-4-(1-hydroxy-1-methylethyl) -2-propylimidazole-5-carboxylic acid). The reaction is illustrated below with chemical formulas. ##STR29##

後処理

  1. customInto a 500-ml flask equipped with a reflux condenser
  2. customthermometer and stirrer were placed
  3. temperatureThe mixture was heated
  4. customa reaction for 24 hours
  5. customAfter completion of the reaction
  6. temperaturethe reaction mixture was cooled to room temperature
  7. stirring' stirring at room temperature
  8. washThe aqueous layer was washed
  9. additionfractionated with the addition of 103 ml of toluene
  10. customto separate out crystals, which
  11. filtrationwere collected by filtration
  12. customdried
  13. temperatureThe crystals were heated
  14. washwashed with methanol
  15. stirringwith stirring
  16. temperaturecooled
  17. filtrationfiltered for collection
  18. customdried

出典と根拠

ORDレコード
ord-e4829d7eea2e4f4e900ca4c0584ff59d
出典データセット
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06040454

反応ノート

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