Triethylamine → HCID 178446283, 화합물

HRID 616251노트

반응식

HRID 616251 반응식
[NH2:1][C:2]1[N:7]=[C:6](Cl)[C:5]([N+:9]([O-:11])=[O:10])=[C:4]([OH:12])[N:3]=1.Cl.[NH2:14][C:15]([CH2:23][CH3:24])([CH2:21][CH3:22])[C:16](=[N:19][OH:20])[CH2:17][OH:18].C(N(CC)CC)C>C(O)C>[NH2:1][C:2]1[N:3]=[C:4]([OH:12])[C:5]([N+:9]([O-:11])=[O:10])=[C:6]([NH:14][C:15]([CH2:23][CH3:24])([CH2:21][CH3:22])[C:16](=[N:19][OH:20])[CH2:17][OH:18])[N:7]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 737620833-Amino-3-ethyl-1-hydroxy-pentan-2-one oxime hydrochlorideHCID 178418667HCID 178418667, 화합물

생성물 1

HCID 178446283HCID 178446283, 화합물수율 48.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A suspension of 2-amino-4-chloro-6-hydroxy-5-nitropyrimidine (III) (Hal=Cl) (2.3 g) in dry ethanol was treated with 3-amino-1-hydroxy-3-spirocyclohexylpropan-2-one oxime hydrochloride (IV) (2.5g) and dry triethylamine (2.7 g) and the mixture was refluxed for 7 h. The reaction mixture was filtered and the solid washed with hot ethanol. The solvent was removed from the filtrate and the resulting yellow oil was triturated with cold water giving a yellow solid which on recrystallisation from water in the presence of charcoal gave the nitropyrimidine (II) (1.85 g; yield 47.4%) as an off-white powder, m.pt >300° (decomp.).

후처리

  1. temperaturethe mixture was refluxed for 7 h
  2. filtrationThe reaction mixture was filtered
  3. washthe solid washed with hot ethanol
  4. customThe solvent was removed from the filtrate
  5. customthe resulting yellow oil was triturated with cold water giving a yellow solid which
  6. customon recrystallisation from water in the presence of charcoal

출처 및 근거

ORD 기록
ord-13acd8104d604aac909e38f8259b518f
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04073786

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