Ethyl 4-hydroxymethyl-2-propyl-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate → HCID 178440150、化合物

HRID 52906ノート

反応式

HRID 52906 の反応式
[OH:1][CH2:2][C:3]1[N:4]=[C:5]([CH2:50][CH2:51][CH3:52])[N:6]([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[C:26]3[N:30](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:29]=[N:28][N:27]=3)=[CH:16][CH:15]=2)[C:7]=1[C:8]([O:10][CH2:11][CH3:12])=[O:9]>C(O)(=O)C>[OH:1][CH2:2][C:3]1[N:4]=[C:5]([CH2:50][CH2:51][CH3:52])[N:6]([CH2:13][C:14]2[CH:15]=[CH:16][C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[C:26]3[NH:30][N:29]=[N:28][N:27]=3)=[CH:18][CH:19]=2)[C:7]=1[C:8]([O:10][CH2:11][CH3:12])=[O:9]

参加物

3

反応物 1

HCID 19036205Ethyl 4-hydroxymethyl-2-propyl-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate

生成物 1

HCID 178440150HCID 178440150、化合物収率 110.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 0.28 g of ethyl 4-hydroxymethyl-2-propyl-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate [prepared as described in step (b) above] in 4 ml of 75% v/v aqueous acetic acid was stirred at 60° C. for 2 hours. The reaction mixture was then concentrated by evaporation under reduced pressure, and the residue was dissolved in toluene. The resulting solution was again concentrated by evaporation under reduced pressure, to remove as much water and acetic acid as possible. The residue was then purified by column chromatography through silica gel, using 9:1 and 4:1 by volume mixtures of methylene chloride and methanol as the eluent, to give 0.20 g of the title compound as an amorphous solid.

後処理

  1. concentrationThe reaction mixture was then concentrated by evaporation under reduced pressure
  2. dissolutionthe residue was dissolved in toluene
  3. concentrationThe resulting solution was again concentrated by evaporation under reduced pressure
  4. customto remove as much water and acetic acid as possible
  5. customThe residue was then purified by column chromatography through silica gel

出典と根拠

ORDレコード
ord-dea9f34729ea4632933ce4e1c591d768
出典データセット
uspto-grants-1997_04
特許番号
US05616599

反応ノート

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