Triethylamine → HCID 178456876, 화합물

HRID 1580591노트

반응식

HRID 1580591 반응식
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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 867329813-Amino-1-phenoxy-3-methylbutan-2-one oxime hydrochlorideHCID 178418667HCID 178418667, 화합물

생성물 1

HCID 178456876HCID 178456876, 화합물수율 16.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.).

후처리

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

출처 및 근거

ORD 기록
ord-d130ce69d23d49ad873b00c5c03e6964
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03933820

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