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Guanidine Hydrochloride → HCID 178459352、化合物

HRID 2390755
ノート
印刷プレビュー

反応式

HRID 2390755 の反応式
Cl.[NH2:2][C:3]([NH2:5])=[NH:4].[F:6][C:7]1[CH:14]=[CH:13][C:10]([CH:11]=O)=[CH:9][CH:8]=1.[CH3:15][CH:16]([CH3:26])[C:17](=O)[CH2:18][C:19]([O:21][CH:22]([CH3:24])[CH3:23])=[O:20].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[NH2:4][C:3]1[NH:5][CH:17]([CH:16]([CH3:26])[CH3:15])[C:18]([C:19]([O:21][CH:22]([CH3:23])[CH3:24])=[O:20])=[C:11]([C:10]2[CH:13]=[CH:14][C:7]([F:6])=[CH:8][CH:9]=2)[N:2]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 57643949Propan-2-yl 4-methyl-3-oxopentanoate

生成物 1

HCID 178459352HCID 178459352、化合物収率 67%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

反応条件

温度
70 °C

実験手順

Guanidine hydrochloride (12.1 g), 4-Fluorobenzaldehyde (7.0 g), isopropyl 4-methyl-3-oxo-pentanoate (8.9 g) and DMF (150 ml) were charged to a vessel equipped with a condenser and connected to a nitrogen line. The resultant mixture was stirred until a clear solution was obtained. Potassium carbonate (17.5 g) was charged and the mixture heated to 70° C. for 3 hours. The reaction mixture was cooled to ambient temperature, filtered, and the solvents removed by evaporation under reduced pressure. The resultant oil was triturated in water at 80° C. and cooled to give a slurry that was filtered and dried to give isopropyl 2-amino-4-(4-fluorophenyl)-6-isopropyl-1,6-dihydropyrimidine-5-carboxylate in 67% yield.

後処理

  1. customequipped with a condenser
  2. customwas obtained
  3. temperatureThe reaction mixture was cooled to ambient temperature
  4. filtrationfiltered
  5. customthe solvents removed by evaporation under reduced pressure
  6. customThe resultant oil was triturated in water at 80° C.
  7. temperaturecooled
  8. customto give a slurry that
  9. filtrationwas filtered
  10. customdried

出典と根拠

ORDレコード
ord-d642ff88a9524c12b12105f6f92ba98d
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273878B2

反応ノート

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