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Triethylamine → HCID 20267949, 화합물

HRID 1719244
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HRID 1719244 반응식
[CH3:1][S:2][C:3]1[N:8]=[C:7]([CH3:9])[C:6]([CH2:10][O:11][CH2:12]Cl)=[CH:5][N:4]=1.Cl.[Cl:15][C:16]1[CH:17]=[N:18][C:19](=[O:22])[NH:20][CH:21]=1.C(N(CC)CC)C>ClCCl>[CH3:1][S:2][C:3]1[N:8]=[C:7]([CH3:9])[C:6]([CH2:10][O:11][CH2:12][N:20]2[CH:21]=[C:16]([Cl:15])[CH:17]=[N:18][C:19]2=[O:22])=[CH:5][N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 126485235-Chloropyrimidin-2-ol hydrochlorideHCID 202679405-[(Chloromethoxy)methyl]-4-methyl-2-(methylsulfanyl)pyrimidine

생성물 1

HCID 20267949HCID 20267949, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

2-Methylthio-4-methyl-5-(chloromethyloxymethyl)pyrimidine (see Preparation 11) (2.7 mmol) in dichloromethane (5 ml) was added dropwise with stirring at room temperature to a solution of 5-chloropyrimidin-2-one hydrochloride (2.7 mmol) and triethylamine in dichloromethane (0.76 ml). The mixture was stirred for 24 hours at room temperature before the solvent was distilled off. The residue was triturated with water, extracted into chloroform and the dried (MgSO4) solution evaporated. yield 0.55 g (65%). 1H NMR (CDCl3): δ2.42 (4-Me), 2.55 (SMe), 4.65 (CH2Pyr), 5.32 (CH2O), 7.80 and 8.42 (H-4, H-6, J 3 Hz), 8.20 (H-6').

후처리

  1. distillationwas distilled off
  2. customThe residue was triturated with water
  3. extractionextracted into chloroform
  4. dry with materialthe dried (MgSO4) solution
  5. customevaporated

출처 및 근거

ORD 기록
ord-7f9e2a72fd784b12b8c6742cf18ca2ba
출처 데이터셋
uspto-grants-1985_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04539324

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