Ammonium Carbonate → 2-[(4-Carbamimidoyl-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carboxylic acid [2-(4-amino-butylcarbamoyl)-ethyl]phenyl-amide

HRID 574109ノート

反応式

HRID 574109 の反応式
C(OC(=O)[NH:7][CH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:13](=[O:45])[CH2:14][CH2:15][N:16]([C:23]([C:25]1[CH:44]=[CH:43][C:28]2[N:29]([CH3:42])[C:30]([CH2:32][NH:33][C:34]3[CH:39]=[CH:38][C:37]([C:40]#[N:41])=[CH:36][CH:35]=3)=[N:31][C:27]=2[CH:26]=1)=[O:24])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)(C)(C)C.C(=O)([O-])[O-].[NH4+:51].[NH4+]>Cl.C(O)C>[NH2:7][CH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]([CH2:14][CH2:15][N:16]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:23]([C:25]1[CH:44]=[CH:43][C:28]2[N:29]([CH3:42])[C:30]([CH2:32][NH:33][C:34]3[CH:39]=[CH:38][C:37]([C:40](=[NH:41])[NH2:51])=[CH:36][CH:35]=3)=[N:31][C:27]=2[CH:26]=1)=[O:24])=[O:45]

参加物

5

反応物 2

HCID 517111Ammonium CarbonateHCID 66706504{4-[3-({2-[(4-Cyano-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carbonyl}-phenyl-amino)-propionylamino]-butyl}-carbamic acid tert-butyl ester

生成物 1

HCID 533274672-[(4-Carbamimidoyl-phenylamino)-methyl]-1-methyl-1H-benzoimidazole-5-carboxylic acid [2-(4-amino-butylcarbamoyl)-ethyl]phenyl-amide

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

The product of 1f (4.81 mmol) was dissolved in a saturated solution of HCl in ethanol (250 mL), the mixture stirred at room temperature over night and then evaporated to dryness at 30° C. The remaining raw material was dissolved in 200 mL dry ethanol, then ammonium carbonate (48.1 mmol) was added and the mixture stirred at room temperature over night. After evaporation of the solvent the remaining raw material was triturated with ca. 5 mL ethanol, the undissolved material separated by filtration and the solvent evaporated at 30° C. The product was then dissolved in 30 mL water, the solution stirred with ca.2g charcoal, filtered and evaporated to dryness.

後処理

  1. customevaporated to dryness at 30° C
  2. dissolutionThe remaining raw material was dissolved in 200 mL dry ethanol
  3. stirringthe mixture stirred at room temperature over night
  4. customAfter evaporation of the solvent the remaining raw material
  5. customwas triturated with ca. 5 mL ethanol
  6. customthe undissolved material separated by filtration
  7. customthe solvent evaporated at 30° C
  8. dissolutionThe product was then dissolved in 30 mL water
  9. stirringthe solution stirred with ca.2g charcoal
  10. filtrationfiltered
  11. customevaporated to dryness

出典と根拠

ORDレコード
ord-5efca9c19a9744dd9e8e0a9593a12f67
出典データセット
uspto-grants-2015_05
特許番号
US09034822B2

反応ノート

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