Hydrazine hydrate (1:1) → alpha-[2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetohydrazide

HRID 1198910ノート

反応式

HRID 1198910 の反応式
[Cl:1][C:2]1[CH:14]=[C:13]([C:15]2[CH:16]([CH3:22])[NH:17][C:18](=[O:21])[NH:19][N:20]=2)[CH:12]=[CH:11][C:3]=1[O:4][CH2:5][C:6](OCC)=[O:7].O.[NH2:24][NH2:25]>C(O)C>[Cl:1][C:2]1[CH:14]=[C:13]([C:15]2[CH:16]([CH3:22])[NH:17][C:18](=[O:21])[NH:19][N:20]=2)[CH:12]=[CH:11][C:3]=1[O:4][CH2:5][C:6]([NH:24][NH2:25])=[O:7]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 14370696Ethyl alpha-[2-chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetate

生成物 1

HCID 14370703alpha-[2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetohydrazide収率 76.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 1.0 g of ethyl α-[2-chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetate (prepared as described in Example 5) and 0.39 g of 80% hydrazine hydrate in 10 ml of ethanol was stirred on an oil bath kept at 105° C. for 4 hours. The mixture was then cooled, after which the crystals which precipitated were collected by filtration and recrystallized from ethanol, to give 0.73 g of the title compound as white crystals melting at 252°-254° C.

後処理

  1. temperatureThe mixture was then cooled
  2. customafter which the crystals which precipitated
  3. filtrationwere collected by filtration
  4. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-f9a4718fc6454e47b7b43ea5fc2fd283
出典データセット
uspto-grants-1990_02
特許番号
US04898862

反応ノート

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