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Triethylamine → HCID 14835675、化合物

HRID 1709242
ノート
印刷プレビュー

反応式

HRID 1709242 の反応式
[CH3:1][O:2][CH:3]([O:13][CH3:14])[C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7](O)=[O:8].C(N(CC)CC)C.C(Cl)(=O)OCC.O.[NH2:29][NH2:30]>C(Cl)Cl>[CH3:1][O:2][CH:3]([O:13][CH3:14])[C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([NH:29][NH2:30])=[O:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 24654Hydrazine hydrate (1:1)HCID 148356743-(Dimethoxymethyl)benzoic acid

生成物 1

HCID 14835675HCID 14835675、化合物収率 98.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-55 °C

実験手順

3.92 g of 3-dimethoxymethylbenzoic acid and 2.22 g of triethylamine were dissolved in 40 ml of methylene chloride. To the solution was dropwise added 2.28 g of ethyl chlorocarbonate at -30° to -20° C. The mixture was stirred for 30 minutes at the same temperature. The mixture was then cooled to -55° C., and 5.00 g of hydrazine hydrate was added thereto. The temperature of the mixture was elevated to room temperature. The methylene chloride layer was separated, washed with water and a saturated aqueous sodium chloride solution in this order and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue was purified by a column chromatography (eluant: chloroform/ethanol=30/1) to obtain 4.13 g of colorless oily 3-dimethoxymethylbenzhydrazide.

後処理

  1. customat -30° to -20° C
  2. customwas elevated to room temperature
  3. customThe methylene chloride layer was separated
  4. washwashed with water
  5. dry with materiala saturated aqueous sodium chloride solution in this order and dried over anhydrous magnesium sulfate
  6. customThe solvent was removed by distillation under reduced pressure
  7. customThe residue was purified by a column chromatography (eluant: chloroform/ethanol=30/1)

出典と根拠

ORDレコード
ord-18ef36b78ea44a8d85845e99928a62e3
出典データセット
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04948796

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート