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Triethylamine → Ethyl 2-[4-(3-isopropyl-4-methoxybenzyl)-3,5-dimethylanilino]-2-oxoacetate

HRID 392892
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HRID 392892 반응식
[CH:1]([C:4]1[CH:5]=[C:6]([CH:17]=[CH:18][C:19]=1[O:20][CH3:21])[CH2:7][C:8]1[C:14]([CH3:15])=[CH:13][C:11]([NH2:12])=[CH:10][C:9]=1[CH3:16])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:29](Cl)([C:31]([O:33][CH2:34][CH3:35])=[O:32])=[O:30]>ClCCl>[CH:1]([C:4]1[CH:5]=[C:6]([CH:17]=[CH:18][C:19]=1[O:20][CH3:21])[CH2:7][C:8]1[C:9]([CH3:16])=[CH:10][C:11]([NH:12][C:29](=[O:30])[C:31]([O:33][CH2:34][CH3:35])=[O:32])=[CH:13][C:14]=1[CH3:15])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 112890854-(3-Isopropyl-4-methoxybenzyl)-3,5-dimethylaniline

생성물 1

HCID 10110509Ethyl 2-[4-(3-isopropyl-4-methoxybenzyl)-3,5-dimethylanilino]-2-oxoacetate수율 38.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

246 mg (0.86 mmol) of 4-(3-isopropyl-4-methoxybenzyl)-3,5-dimethylaniline (Example VII) are dissolved with 97 mg (0.96 mmol) of triethylamine in 10 ml of dichloromethane, and 160 mg (1.17 mmol) of ethoxalyl chloride are added dropwise. The mixture is stirred at room temperature for 4 hours, washed with sodium bicarbonate solution and water and dried over sodium sulphate, and the solvent is removed in vacuo. Purification by chromatography affords 128 mg (38%) of ethyl 2-[4-(3-isopropyl-4-methoxybenzyl)-3,5-dimethylanilino]-2-oxoacetate.

후처리

  1. additionare added dropwise
  2. washwashed with sodium bicarbonate solution and water
  3. dry with materialdried over sodium sulphate
  4. customthe solvent is removed in vacuo
  5. customPurification by chromatography

출처 및 근거

ORD 기록
ord-19324026a4f0434ebeee230cd523f0d6
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06803480B2

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