Triethylamine → HCID 178446283、化合物

HRID 616251ノート

反応式

HRID 616251 の反応式
[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

参加物

5

反応物 3

HCID 8471TriethylamineHCID 737620833-Amino-3-ethyl-1-hydroxy-pentan-2-one oxime hydrochlorideHCID 178418667HCID 178418667、化合物

生成物 1

HCID 178446283HCID 178446283、化合物収率 48.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-13acd8104d604aac909e38f8259b518f
出典データセット
uspto-grants-1978_02
特許番号
US04073786

反応ノート

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