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Potassium Carbonate → HCID 178429432, 화합물

HRID 577043
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HRID 577043 반응식
[CH3:1][C:2]1[N:7]=[C:6]([SH:8])[N:5]=[C:4]([OH:9])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[Br:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23]Br)[C:18]=1[Cl:25]>CN(C=O)C>[Br:16][C:17]1[C:18]([Cl:25])=[C:19]([CH2:23][S:8][C:6]2[N:5]=[C:4]([OH:9])[CH:3]=[C:2]([CH3:1])[N:7]=2)[CH:20]=[CH:21][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 223242561-Bromo-3-(bromomethyl)-2-chlorobenzeneHCID 178429541HCID 178429541, 화합물

생성물 1

HCID 178429432HCID 178429432, 화합물수율 78%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

6-methyl-2-sulfanylpyrimidin-4-ol (1.21 g, 8.5 mmol) was dissolved in anhydrous DMF (50 mL), and then potassium carbonate (1.76 g, 12.7 mmol) and 1-bromo-3-(bromomethyl)-2-chlorobenzene (3.13 g, 11.0 mmol) in anhydrous DMF (10 mL) were added. The mixture was stirred overnight at room temperature. The solid was filtered, washed with water plus diethyl ether, and dried in vacuo to afford to 2-{[(3-bromo-2-chlorophenyl)methyl]sulfanyl}-6-methylpyrimidin-4-ol (2.28 g, 78% yield); 1H NMR (400 MHz, DMSO-d6): δ 2.03 (s, 3H), 4.39 (s, 2H), 5.67 (s, 1H), 7.17 (t, J=7.9 Hz, 1H), 7.63 (d, J=7.9 Hz, 2H); LRMS (ES+) m/z 345 (75%, M+1), 347 (100%, M+3), 349 (30%, M+5).

후처리

  1. filtrationThe solid was filtered
  2. washwashed with water plus diethyl ether
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-67130c96f1ef486dbd4b68d02c30edcd
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040538B2

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