HCID 21472721, 화합물 → HCID 69945089, 화합물

HRID 2295058노트

반응식

HRID 2295058 반응식
C(OC([N:8]1[C:12]2[C:13]([F:25])=[CH:14][C:15]([NH:18]C(NCCN)=S)=[C:16]([CH3:17])[C:11]=2[N:10]=[CH:9]1)=O)(C)(C)C>CO>[F:25][C:13]1[C:12]2[N:8]=[CH:9][NH:10][C:11]=2[C:16]([CH3:17])=[C:15]([NH:18][N:10]2[CH2:11][CH2:12][N:8]=[CH:9]2)[CH:14]=1

참가 물질

3

반응물 1

HCID 21472721HCID 21472721, 화합물

생성물 1

HCID 69945089HCID 69945089, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of N-(1-tert-butoxycarbonyl-7-fluoro-4-methyl-5-benzimidazolyl)-N'-2-aminoethylthio-urea (0.5 g) and mercuric acetate (0.52 g) in methanol (150 mL) is stirred at room temperature for 1 hour. The resulting black mixture is filtered on Celite with methanol wash of the solids. The filtrate is rotary evaporated and the residue filtered through a short pad of silica gel, eluting 25% methanol in chloroform containing 1% of ammonium hydroxide. The product-containing fractions are rotary evaporated, the residue diluted with water (15 mL), filtered through a plug of glass wool and lyophilized to afford 7-fluoro-4-methyl-5-(2-imidazolinylamino)benzimidazole as a pale yellow solid.

후처리

  1. filtrationThe resulting black mixture is filtered on Celite with methanol
  2. washwash of the solids
  3. customThe filtrate is rotary evaporated
  4. filtrationthe residue filtered through a short pad of silica gel
  5. washeluting 25% methanol in chloroform containing 1% of ammonium hydroxide
  6. additionthe residue diluted with water (15 mL)
  7. filtrationfiltered through a plug of glass wool

출처 및 근거

ORD 기록
ord-c10720456dd54c2f8c6f9f36bbd4924d
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05691370

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