HCID 21472721、化合物 → HCID 69945089、化合物

HRID 2260741ノート

反応式

HRID 2260741 の反応式
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

参加物

3

反応物 1

HCID 21472721HCID 21472721、化合物

生成物 1

HCID 69945089HCID 69945089、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of N-(1-tert-butoxycarbonyl-7-fluoro-4-methyl-5-benzimidazolyl)-N'-2-aminoethylthiourea (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 shod 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.

後処理

  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 shod 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

出典と根拠

ORDレコード
ord-e8aa27b9a3ba48d1998d24ed376fd77e
出典データセット
uspto-grants-1995_12
特許番号
US05478858

反応ノート

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