Acetic Acid → HCID 178433372、化合物

HRID 445052ノート

反応式

HRID 445052 の反応式
[C:1]([CH2:3][C:4]1[CH:18]=[CH:17][C:7]([CH2:8][CH:9]([C:14](=O)[CH3:15])[C:10](OC)=[O:11])=[CH:6][CH:5]=1)#[N:2].C(=O)(O)O.[NH2:23][C:24]([NH2:26])=[NH:25].C(O)(=O)C>CO.O>[NH2:26][C:24]1[N:25]=[C:10]([OH:11])[C:9]([CH2:8][C:7]2[CH:17]=[CH:18][C:4]([CH2:3][C:1]#[N:2])=[CH:5][CH:6]=2)=[C:14]([CH3:15])[N:23]=1

参加物

6

反応物 3

HCID 176Acetic AcidHCID 286947Carbonic acid-guanidine (1:1)HCID 59590640Methyl 2-(4-(cyanomethyl)benzyl)-3-oxobutanoate

生成物 1

HCID 178433372HCID 178433372、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
30 °C

実験手順

A stirred mixture of the crude product from step (i) and guanidine carbonate (36.7 g, 0.20 mol) in methanol (389 g) was heated under reflux for 7 hours. The mixture was cooled to 30° C., diluted with water (222 g), and the pH of the solution was adjusted to pH 6.5 with acetic acid. After the mixture was cooled to 5° C., the resulting precipitate was collected by filtration, washed with methanol twice (167 g, 333 g), and dried under reduced pressure to give the subtitle compound as a solid, 32.6 g.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 7 hours
  3. temperatureAfter the mixture was cooled to 5° C.
  4. filtrationthe resulting precipitate was collected by filtration
  5. washwashed with methanol twice (167 g, 333 g)
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-7c417083a22c462e8fcf15d1827633ac
出典データセット
uspto-grants-2013_07
特許番号
US08476288B2

反応ノート

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