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

HRID 1617160ノート

反応式

HRID 1617160 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-66d9c34f951b424ebc17433fa66c3697
出典データセット
uspto-grants-2014_07
特許番号
US08765939B2

反応ノート

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