1,3-Dichloroacetone → HCID 178455314, 화합물

HRID 1873568

반응식

HRID 1873568 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH2:11])=[S:10])=[CH:4][CH:3]=1.Cl[CH2:13][C:14]([CH2:16]Cl)=O.[NH2:18][C:19]1[C:24]([C:25]#[N:26])=[C:23]([CH:27]2[CH2:32][CH2:31][CH:30]([O:33][Si:34]([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:36])[CH3:35])[CH2:29][CH2:28]2)[C:22]([C:41]#[N:42])=[C:21]([SH:43])[N:20]=1.C(=O)(O)[O-].[Na+]>CN(C=O)C>[NH2:18][C:19]1[C:24]([C:25]#[N:26])=[C:23]([C@H:27]2[CH2:28][CH2:29][C@@H:30]([O:33][Si:34]([C:37]([CH3:39])([CH3:40])[CH3:38])([CH3:35])[CH3:36])[CH2:31][CH2:32]2)[C:22]([C:41]#[N:42])=[C:21]([S:43][CH2:16][C:14]2[N:11]=[C:9]([NH:8][C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=3)[S:10][CH:13]=2)[N:20]=1

참가 물질

6

반응물 4

HCID 107931,3-DichloroacetoneHCID 516892Sodium BicarbonateHCID 6930614-FluorophenylthioureaHCID 1784550312-Amino-4-(4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-6-mercaptopyridine-3,5-dicarbonitrile

생성물 1

HCID 178455314HCID 178455314, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

43 mg (0.26 mmol) of 4-fluorophenylthiourea and 31 mg (0.24 mmol) of 1,3-dichloroacetone are dissolved in 2 ml DMF and stirred at +80° C. for 3 h. After cooling to RT 93 mg (0.23 mmol) of the compound from Example 12A (cis isomer) and 78 mg (0.93 mmol) of sodium bicarbonate are added, and the reaction mixture is stirred at RT for 20 h. The mixture is then directly purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5).

후처리

  1. additionare added
  2. stirringthe reaction mixture is stirred at RT for 20 h
  3. customThe mixture is then directly purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)

출처 및 근거

ORD 기록
ord-bf5776ccca9143d58fd8430e59cbccb4
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08304412B2

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