Ammonia → 2,5'-Bi-1H-benzimidazole, 1-methyl-2'-propyl-

HRID 2292717노트

반응식

HRID 2292717 반응식
S(O)(O)(=O)=O.[CH2:6]([C:9]1[NH:10][C:11]2[CH:17]=[C:16]([C:18](O)=O)[CH:15]=[CH:14][C:12]=2[N:13]=1)[CH2:7][CH3:8].C([C:24]1[NH:25][C:26]2[CH:32]=[C:31](C(O)=O)[CH:30]=[CH:29][C:27]=2[N:28]=1)CC.Cl.Cl.CNC1C=CC=CC=1N.N>O>[CH2:6]([C:9]1[NH:10][C:11]2[CH:17]=[C:16]([C:18]3[N:25]([CH3:24])[C:26]4[CH:32]=[CH:31][CH:30]=[CH:29][C:27]=4[N:28]=3)[CH:15]=[CH:14][C:12]=2[N:13]=1)[CH2:7][CH3:8]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 91296N-Methyl-o-phenylenediamine dihydrochlorideHCID 856442212-n-Propyl-benzimidazole-5-carboxylic acid-hemisulphate

생성물 1

HCID 104694762,5'-Bi-1H-benzimidazole, 1-methyl-2'-propyl-

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 6.7 g (25 mMol) of 2-n-propyl-benzimidazole-5-carboxylic acid-hemisulphate and 4.9 g (25 mMol) of 2-methylaminoaniline-dihydrochloride in 200 g of polyphosphoric acid is stirred for 5 hours at 150° C., then poured onto 600 ml of water and made alkaline with concentrated ammonia whilst cooling with ice. The resulting solution is extracted three times with 200 ml of ethyl acetate, the crude product thus obtained is purified by column chromatography (300 g of silica gel; eluant: methylene chloride/methanol=15:1).

후처리

  1. temperaturewhilst cooling with ice
  2. extractionThe resulting solution is extracted three times with 200 ml of ethyl acetate

출처 및 근거

ORD 기록
ord-859b6e201805402fb07780c425093ede
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05684029

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