4-Methylamino-3-chloracetamidobenzoic acid-n-(n-propyl)-n-(2-ethoxycarbonylethyl)amide → 2-Chloromethyl-1-methylbenzimidazol-5-yl-carboxylic acid-n-(n-propyl)-n-(2-ethoxycarbonylethyl)amide

HRID 2288362

反応式

HRID 2288362 の反応式
[CH2:1]([N:4]([CH2:20][CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:5](=[O:19])[C:6]1[CH:11]=[CH:10][C:9]([NH:12][CH3:13])=[C:8]([NH:14][C:15](=O)[CH2:16][Cl:17])[CH:7]=1)[CH2:2][CH3:3]>C(O)(=O)C>[CH2:1]([N:4]([CH2:20][CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:5]([C:6]1[CH:11]=[CH:10][C:9]2[N:12]([CH3:13])[C:15]([CH2:16][Cl:17])=[N:14][C:8]=2[CH:7]=1)=[O:19])[CH2:2][CH3:3]

参加物

3

反応物 1

HCID 184124094-Methylamino-3-chloracetamidobenzoic acid-n-(n-propyl)-n-(2-ethoxycarbonylethyl)amide

生成物 1

HCID 184123762-Chloromethyl-1-methylbenzimidazol-5-yl-carboxylic acid-n-(n-propyl)-n-(2-ethoxycarbonylethyl)amide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

1.6 g (4.3 mMol) of 4-methylamino-3-chloracetamido-benzoic acid-N-(n-propyl)-N-(2-ethoxycarbonylethyl)-amide were heated to 100° C. in 25 ml of acetic acid for 30 minutes. Then the solvent was distilled off, the crude product was taken up in 40 ml methylene chloride/ethanol (9:1) and washed with 20 ml saturated sodium hydrogen carbonate solution. The organic phase was dried with sodium sulphate and evaporated down. Yield: 1.5 g (100% of theory) of brown oil, Rf value: 0.63 (silica gel; ethyl acetate/ethanol/ammonia =90:10:1)

後処理

  1. distillationThen the solvent was distilled off
  2. washwashed with 20 ml saturated sodium hydrogen carbonate solution
  3. dry with materialThe organic phase was dried with sodium sulphate
  4. customevaporated down

出典と根拠

ORDレコード
ord-d2ac45776610487695402fea17528042
出典データセット
uspto-grants-2000_07
特許番号
US06087380

関連ノート

読み込み中…