Carbonic acid-guanidine (1:1) → HCID 178497677、化合物

HRID 2387814ノート

反応式

HRID 2387814 の反応式
C(=O)(O)O.[NH2:5][C:6]([NH2:8])=[NH:7].C([O:11][C:12]([CH:14]([C:27](=O)[CH3:28])[CH2:15][C:16]1[CH:25]=[CH:24][C:19]([C:20]([O:22][CH3:23])=[O:21])=[CH:18][C:17]=1[F:26])=O)C>CO>[NH2:7][C:6]1[N:8]=[C:12]([OH:11])[C:14]([CH2:15][C:16]2[CH:25]=[CH:24][C:19]([C:20]([O:22][CH3:23])=[O:21])=[CH:18][C:17]=2[F:26])=[C:27]([CH3:28])[N:5]=1

参加物

4

反応物 2

HCID 286947Carbonic acid-guanidine (1:1)HCID 68412608Methyl 4-(2-(ethoxycarbonyl)-3-oxobutyl)-3-fluorobenzoate

生成物 1

HCID 178497677HCID 178497677、化合物収率 60.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

Guanidine carbonate (6.86 g) was added to a stirred solution of the product from step (i) (11.1 g) in MeOH (200 mL). The resulting mixture was stirred at 70° C. for 15 h. The mixture was allowed to cool to rt and the resulting precipitate collected by filtration. The solid was suspended in water (50 mL), collected by filtration and washed with MeOH to give the subtitle compound as a colourless solid 6.60 g that was used without further purification.

後処理

  1. temperatureto cool to rt
  2. filtrationthe resulting precipitate collected by filtration
  3. filtrationcollected by filtration
  4. washwashed with MeOH

出典と根拠

ORDレコード
ord-25546e251f804d639b02d5cec2ac73c1
出典データセット
uspto-grants-2012_09
特許番号
US08268990B2

反応ノート

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