Trimethyl orthoacetate → HCID 14232984、化合物

HRID 580475ノート

反応式

HRID 580475 の反応式
[NH2:1][C:2]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][CH2:9][N:10]1[CH:14]=[CH:13][N:12]=[CH:11]1)=[O:5].[C:20](OC)(OC)(OC)[CH3:21]>C(O)C>[Cl:19][C:16]1[CH:15]=[C:3]2[C:2](=[CH:18][CH:17]=1)[N:1]=[C:20]([CH3:21])[N:6]([CH2:7][CH2:8][CH2:9][N:10]1[CH:14]=[CH:13][N:12]=[CH:11]1)[C:4]2=[O:5]

参加物

4

反応物 2

HCID 15050Trimethyl orthoacetateHCID 135889602-Amino-5-chloro-N-[3-(1H-imidazol-1-yl)propyl]benzamide

生成物 1

HCID 14232984HCID 14232984、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2.79 g of 2-amino-5-chloro-N-[3-(1H-imidazol-1-yl)propyl]benzamide, 5 ml of trimethyl orthoacetate and 10 ml of ethyl alcohol was heated at reflux for 24 hours. The resulting solution was concentrated and the residue was triturated with ether and gave a solid. The ether was decanted and the solid was dissolved in ethyl acetate and allowed to stand. The precipitate was collected and gave 650 mg of the desired product as tan crystals, mp 190°-192° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 24 hours
  3. concentrationThe resulting solution was concentrated
  4. customthe residue was triturated with ether
  5. customgave a solid
  6. customThe ether was decanted
  7. dissolutionthe solid was dissolved in ethyl acetate
  8. customThe precipitate was collected

出典と根拠

ORDレコード
ord-76e94dc9143d4c568ba86cd50c6e953a
出典データセット
uspto-grants-1988_06
特許番号
US04753944

反応ノート

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