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

HRID 52906노트

반응식

HRID 52906 반응식
[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]

참가 물질

3

반응물 1

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

생성물 1

HCID 178440150HCID 178440150, 화합물수율 110.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dea9f34729ea4632933ce4e1c591d768
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616599

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