Hydrochloric Acid → HCID 178455691, 화합물

HRID 591226노트

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HRID 591226 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 178455691HCID 178455691, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 312751,4-Dioxane용매

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온도
80 °C

실험 절차

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.

후처리

  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%)

출처 및 근거

ORD 기록
ord-083555a2301a4b0ab0362f0529b3cc77
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238653B2

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