Triethylamine → HCID 71145194、化合物

HRID 924600

反応式

HRID 924600 の反応式
[CH2:1]([O:3][C:4]([NH:6][NH2:7])=[O:5])[CH3:2].C(N(CC)CC)C.[CH3:15][C:16]1[CH:21]=[C:20]([CH3:22])[CH:19]=[C:18]([CH3:23])[C:17]=1[CH2:24][C:25](Cl)=[O:26]>O1CCCC1>[CH2:1]([O:3][C:4]([NH:6][NH:7][C:25](=[O:26])[CH2:24][C:17]1[C:16]([CH3:15])=[CH:21][C:20]([CH3:22])=[CH:19][C:18]=1[CH3:23])=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 110307542,4,6-Trimethylbenzeneacetyl chloride

生成物 1

HCID 71145194HCID 71145194、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of hydrazinecarboxylic acid ethyl ester (ethyl carbazate, 32.8 g, 314.9 mmol) and triethylamine (44.1 ml, 32.0 g, 316.4 mmol) in tetrahydrofuran (1000 ml) at 0° C. was added (2,4,6-trimethyl-phenyl)-acetyl chloride (62.0 g, 315.2 mmol) dropwise. The thick suspension was stirred at room temperature for one hour and the solvent evaporated. The residue was suspended in a mixture of t-butyl methyl ether (500 ml) and water (500 ml), stirred, filtered and the solid washed with small portions of water and t-butyl methyl ether. The solid was dried in vacuo over phosphorus pentoxide at 40° C. Yield: 78.4 g of N′-[2-(2,4,6-trimethyl-phenyl)-acetyl]-hydrazinecarboxylic acid ethyl ester as a white solid, mp 184-186° C.

後処理

  1. customthe solvent evaporated
  2. additionThe residue was suspended in a mixture of t-butyl methyl ether (500 ml) and water (500 ml)
  3. stirringstirred
  4. filtrationfiltered
  5. washthe solid washed with small portions of water and t-butyl methyl ether
  6. dry with materialThe solid was dried in vacuo over phosphorus pentoxide at 40° C

出典と根拠

ORDレコード
ord-c27fa7da8c534a81938e2e94d88e8c28
出典データセット
uspto-grants-2016_03
特許番号
US09282743B2

関連ノート

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