Carbonic acid-guanidine (1:1) → HCID 178497677, 화합물

HRID 1617160노트

반응식

HRID 1617160 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 178497677HCID 178497677, 화합물수율 60.5%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-66d9c34f951b424ebc17433fa66c3697
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765939B2

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