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Triethylamine → HCID 14835675, 화합물

HRID 1709242
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HRID 1709242 반응식
[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]
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참가 물질

6

반응물 4

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

생성물 1

HCID 14835675HCID 14835675, 화합물수율 98.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
-55 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-18ef36b78ea44a8d85845e99928a62e3
출처 데이터셋
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04948796

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