Triethylamine → 4-Chloro-5-methoxy-6-(methoxymethyl)pyrimidine

HRID 1378400

반응식

HRID 1378400 반응식
O[C:2]1[C:7]([O:8][CH3:9])=[C:6]([CH2:10][O:11][CH3:12])[N:5]=[CH:4][N:3]=1.C(N(CC)CC)C.P(Cl)(Cl)([Cl:22])=O.C(=O)([O-])[O-].[Na+].[Na+]>ClC(Cl)C>[Cl:22][C:2]1[C:7]([O:8][CH3:9])=[C:6]([CH2:10][O:11][CH3:12])[N:5]=[CH:4][N:3]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 178494688HCID 178494688, 화합물

생성물 1

HCID 152793504-Chloro-5-methoxy-6-(methoxymethyl)pyrimidine

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

반응 조건

온도
80 °C

실험 절차

85.0 g (0.5 mol) of 4-hydroxy-5-methoxy-6-methoxymethylpyrimidine were suspended in 600 ml of dichloroethane, 50.5 g of triethylamine were added, and 260 g (1.7 mol) of phosphorus oxychloride were then added without cooling. The mixture was stirred for 3 hours at 80° C., poured into ice-water and neutralized by adding solid sodium carbonate, the organic phase was separated, and the water phase was extracted several times by stirring with methylene chloride. The combined organic phases were dried and concentrated. The residue was distilled under a water pump vacuum. 66.1 g (70% of theory) of a yellow oil were obtained. B.p. 93°-96° C./0.1mm.

후처리

  1. temperaturewithout cooling
  2. customthe organic phase was separated
  3. extractionthe water phase was extracted several times
  4. stirringby stirring with methylene chloride
  5. customThe combined organic phases were dried
  6. concentrationconcentrated
  7. distillationThe residue was distilled under a water pump vacuum
  8. custom66.1 g (70% of theory) of a yellow oil were obtained

출처 및 근거

ORD 기록
ord-3d4eae15b48d410c83b87577a98525b3
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05668140

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