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Methanesulfonic Acid → HCID 178481675, 화합물

HRID 1091349
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HRID 1091349 반응식
C([O:3][C:4](=O)[CH2:5][C:6]([C:8]1[CH:13]=[CH:12][N:11]=[CH:10][C:9]=1[F:14])=O)C.[CH3:16][NH:17][C:18]([NH2:20])=[S:19].N12CCCN=C1CCCCC2.CS(O)(=O)=O>C1(C)C=CC=CC=1.O>[F:14][C:9]1[CH:10]=[N:11][CH:12]=[CH:13][C:8]=1[C:6]1[N:20]=[C:18]([SH:19])[N:17]([CH3:16])[C:4](=[O:3])[CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6395Methanesulfonic AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 2723704MethylthioureaHCID 59576754Ethyl 3-fluoro-beta-oxo-4-pyridinepropanoate

생성물 1

HCID 178481675HCID 178481675, 화합물수율 68.2%

시약·촉매·용매 2

HCID 962Water
용매
HCID 1140Toluene용매

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온도
100 °C

실험 절차

A suspension of 3-(3-fluoropyridin-4-yl)-3-oxo-propionic acid ethyl ester (60.3 g, 286 mmol), N-methylthiourea (88 g, 976 mmol) and 1,8-diazabicyclo[5,4,0]undec-7-ene (48 g, 315 mmol) in toluene (600 ml) was heated at 100° C. for 5 hour. After addition of water (2000 ml) and methanesulfonic acid (30.3 g, 315 mmol) at room temperature and stirring for one hour, resulting precipitate was collected by filtration and dried to afford 6-(3-fluoropyridin-4-yl)-2-mercapto-3-methyl-3H-pyrimidin-4-one (46.3 g, 195 mmol, 68%) as white crystals.

후처리

  1. customresulting precipitate
  2. filtrationwas collected by filtration
  3. customdried

출처 및 근거

ORD 기록
ord-ee1b90cc631a41bc80863838e2b82034
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08129377B2

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