Hydrochloric Acid → HCID 178455691、化合物

HRID 591226ノート

反応式

HRID 591226 の反応式
[Na].[NH2:2][C:3]1[N:8]([NH2:9])[C:7](=[O:10])[CH:6]=[C:5]([CH3:11])[N:4]=1.[F:12][C:13]([F:21])([CH2:19][CH3:20])[C:14](OCC)=O.Cl>O1CCOCC1.C(O)C>[F:12][C:13]([C:14]1[N:2]=[C:3]2[N:4]=[C:5]([CH3:11])[CH:6]=[C:7]([OH:10])[N:8]2[N:9]=1)([F:21])[CH2:19][CH3:20]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 9131753-Amino-2-imino-6-methyl-2,3-dihydropyrimidin-4(1H)-oneHCID 5360545SodiumHCID 22749276Ethyl 2,2-difluorobutanoate

生成物 1

HCID 178455691HCID 178455691、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

To a solution of NaEtO prepared from sodium (FLUKA, 0.152 g, 6.62 mmol) and ethanol (25 mL), Intermediate 1 (0.773 g, 5.52 mmol) was added, and the mixture was heated at 80° C. for 30 min. Then, the reaction was cooled down to room temperature and ethyl 2,2-difluorobutanoate (FLUOROCHEM, 1007 mg, 6.62 mmol) was added and the reaction mixture was stirred at 80° C. for 3 h. A solution of HCl (1.655 mL, 6.62 mmol) in dioxane was added and a white solid was formed. The residue was purified (silica gel column, eluting with DCM:MeOH mixtures from 100:0 to 90:10%) to obtain Intermediate 6 as a white solid.

後処理

  1. additionwas added
  2. temperatureThen, the reaction was cooled down to room temperature
  3. customa white solid was formed
  4. customThe residue was purified
  5. wash(silica gel column, eluting with DCM:MeOH mixtures from 100:0 to 90:10%)

出典と根拠

ORDレコード
ord-083555a2301a4b0ab0362f0529b3cc77
出典データセット
uspto-grants-2016_01
特許番号
US09238653B2

反応ノート

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