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Hydrochloric Acid → HCID 178429461, 화합물

HRID 576967
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HRID 576967 반응식
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:18])[C:7]=1[CH2:8][S:9][C:10]1[N:15]=[C:14]([OH:16])[CH:13]=[C:12]([CH3:17])[N:11]=1.Cl.O1CCOCC1>CO>[ClH:1].[Cl:18][C:6]1[CH:5]=[N:4][CH:3]=[C:2]([Cl:1])[C:7]=1[CH2:8][S:9][C:10]1[N:15]=[C:14]([OH:16])[CH:13]=[C:12]([CH3:17])[N:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 178429460HCID 178429460, 화합물

생성물 1

HCID 178429461HCID 178429461, 화합물수율 146.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2-{[(3,5-dichloropyridin-4-yl)methyl]sulfanyl}-6-methylpyrimidin-4-ol (200 mg, 662 μmol) was stirred in methanol (20 mL) and a solution of 4 N HCl in dioxane (250 μL, 993 mmol) was added dropwise at 0° C. The mixture was stirred for 30 minutes at room temperature (clear solution). The solvent was removed, and the residue was washed 3 times with diethyl ether and dried in vacuo to afford 2-{[(3,5-dichloropyridin-4-yl)methyl]sulfanyl}-6-methylpyrimidin-4-ol hydrochloride (164 mg, 73% yield); 1H NMR (400 MHz, DMSO-d6): δ 2.24 (s, 3H), 4.69 (s, 2H), 6.13 (s, 1H), 8.67 (s, 2H); LRMS (ES+) m/z 302 (100%, M+1), 304 (70%, M+3).

후처리

  1. customThe solvent was removed
  2. washthe residue was washed 3 times with diethyl ether
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-d8891d7c38534bd4a3c51919c482d84d
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040538B2

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