Triethylamine → HCID 178469033, 화합물

HRID 1458647

반응식

HRID 1458647 반응식
Cl[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([CH2:13][CH3:14])[N:5]=[CH:4][N:3]=1.[CH3:15][Si:16]([CH3:25])([CH3:24])[C@@H:17]1[CH2:22][CH2:21][C@H:20]([NH2:23])[CH2:19][CH2:18]1.C(N(CC)CC)C>O.CCl>[CH2:11]([O:10][C:8]([C:7]1[C:2]([NH:23][C@H:20]2[CH2:19][CH2:18][C@@H:17]([Si:16]([CH3:25])([CH3:24])[CH3:15])[CH2:22][CH2:21]2)=[N:3][CH:4]=[N:5][C:6]=1[CH2:13][CH3:14])=[O:9])[CH3:12]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 18357824HCID 18357824, 화합물HCID 178504289HCID 178504289, 화합물

생성물 1

HCID 178469033HCID 178469033, 화합물

시약·촉매·용매 1

HCID 21639426Water methyl chloride용매

실험 절차

1.00 g (4.66 mmol) of 4-chloro-5-ethoxycarbonyl-6-ethylpyrimidine (EP 606 011), 0.84 g (4.89 mmol) of cis-4-trimethylsilylcyclohexylamine and 0.94 g (9.29 mmol) of triethylamine were heated at 70° C. for 5 hours without solvent. After cooling, the mixture was taken up in water/methyl chloride and the organic phase was dried and concentrated. The residue was purified by chromatography on silica gel using petroleum ether/ethyl acetate (4:1), to give 1.1 g (67% of theory) of a colorless oil.

후처리

  1. temperatureAfter cooling
  2. customthe organic phase was dried
  3. concentrationconcentrated
  4. customThe residue was purified by chromatography on silica gel
  5. customto give 1.1 g (67% of theory) of a colorless oil

출처 및 근거

ORD 기록
ord-719b88d13be445cf8f18b959a00fac99
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05852023

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