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Triethylamine → HCID 13066646, 화합물

HRID 1606647
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HRID 1606647 반응식
[C:1]([O:4][C:5]1[CH:24]=[CH:23][CH:22]=[CH:21][C:6]=1[C:7]([NH:9][C:10]1[CH:19]=[C:18]([NH2:20])[CH:17]=[CH:16][C:11]=1[C:12]([O:14][CH3:15])=[O:13])=[O:8])(=[O:3])[CH3:2].[C:25]([O:28][C:29]1[CH:37]=[CH:36][CH:35]=[CH:34][C:30]=1[C:31](Cl)=[O:32])(=[O:27])[CH3:26].C(N(CC)CC)C>O1CCCC1>[C:1]([O:4][C:5]1[CH:24]=[CH:23][CH:22]=[CH:21][C:6]=1[C:7]([NH:9][C:10]1[CH:19]=[C:18]([NH:20][C:31](=[O:32])[C:30]2[CH:34]=[CH:35][CH:36]=[CH:37][C:29]=2[O:28][C:25](=[O:27])[CH3:26])[CH:17]=[CH:16][C:11]=1[C:12]([O:14][CH3:15])=[O:13])=[O:8])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 796682-Acetoxybenzoyl chlorideHCID 21544117HCID 21544117, 화합물

생성물 1

HCID 13066646HCID 13066646, 화합물수율 66.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

In 80 ml of tetrahydrofuran were dissolved 2 g of methyl 2-(2'-acetoxybenzamido)-4-aminobenzoate and 11.8 g of 2-acetoxybenzoylchloride, and to the solution was added dropwise a solution of 0.6 g of triethylamine in 5 ml of tetrahydrofuran while stirring under cooling with ice. Ten minutes after completion of the addition, the mixture was returned to room temperature, followed by stirring at that temperature for one hour. The reaction mixture was then poured into diluted hydrochloric acid-ice to precipitate crystals. The crystals were recovered by filtration and recrystallized from methanol to obtain 2.0 g of methyl 2,4-bis(2'-acetoxybenzamido)-benzoate having a melting point between 143° - 145°C. This product was confirmed to be identical to that obtained in Example 6.

후처리

  1. temperatureunder cooling with ice
  2. additionTen minutes after completion of the addition
  3. customwas returned to room temperature
  4. stirringby stirring at that temperature for one hour
  5. customto precipitate crystals
  6. filtrationThe crystals were recovered by filtration
  7. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-7f2dbb821ff94cf0a076934945ae65e9
출처 데이터셋
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03953496

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