Triethylamine → HCID 178456876、化合物

HRID 1580591ノート

反応式

HRID 1580591 の反応式
Cl.[NH2:2][C:3]([CH3:16])([CH3:15])[C:4](=[N:13][OH:14])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[NH2:17][C:18]1[N:23]=[C:22](Cl)[C:21]([N+:25]([O-:27])=[O:26])=[C:20]([OH:28])[N:19]=1.C(N(CC)CC)C>C(O)C>[NH2:17][C:18]1[N:19]=[C:20]([OH:28])[C:21]([N+:25]([O-:27])=[O:26])=[C:22]([NH:2][C:3]([CH3:16])([CH3:15])[C:4](=[N:13][OH:14])[CH2:5][O:6][C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:23]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 867329813-Amino-1-phenoxy-3-methylbutan-2-one oxime hydrochlorideHCID 178418667HCID 178418667、化合物

生成物 1

HCID 178456876HCID 178456876、化合物収率 16.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 3-amino-1-(p-chloro)-phenoxy-3-methylbutan-2-one oxime hydrochloride (IV) (5.58 g), 2-amino-4-chloro-6-hydroxy-5-nitropyrimidine (III) (Hal = Cl) (3.81 g) and dry triethylamine (8.2 g) was heated to reflux in dry ethanol (240 ml) for 16 hours and filtered hot. The filtrate was reduced in volume and the solid so obtained was filtered off. Recrystallisation from ethanol gave the nitropyrimidine oxime (II) (1.17 g) as a pale yellow gelatinous solid, m.p. >250°C (decomp.).

後処理

  1. temperaturewas heated
  2. filtrationfiltered hot
  3. customthe solid so obtained
  4. filtrationwas filtered off
  5. customRecrystallisation from ethanol

出典と根拠

ORDレコード
ord-d130ce69d23d49ad873b00c5c03e6964
出典データセット
uspto-grants-1976_01
特許番号
US03933820

反応ノート

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