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Triethylamine → HCID 21460722, 화합물

HRID 2396365
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HRID 2396365 반응식
[NH2:1][C:2]1[C:10]2[C:5](=[CH:6][C:7]([Cl:12])=[CH:8][C:9]=2[Cl:11])[NH:4][C:3]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14].[CH2:18](N(CC)CC)C.[F:25][C:26]1[CH:27]=[C:28]([CH:32]=[CH:33][CH:34]=1)[C:29](Cl)=[O:30].C(OCC)(=O)C>C(Cl)Cl>[F:25][C:26]1[CH:27]=[C:28]([CH:32]=[CH:33][CH:34]=1)[C:29](=[O:30])[CH2:18][NH:1][C:2]1[C:10]2[C:5](=[CH:6][C:7]([Cl:12])=[CH:8][C:9]=2[Cl:11])[NH:4][C:3]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 743763-Fluorobenzoyl chlorideHCID 15043966HCID 15043966, 화합물

생성물 1

HCID 21460722HCID 21460722, 화합물수율 81%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Dissolve 3-amino-2-carbethoxy-4,6-dichloroindole (1.09 g, 4 mmol) in methylene chloride (25 mL) and add triethylamine (0.578 mL, 4 mmol) followed by m-fluorobenzoyl chloride (0.488 mL, 4 mmol). Stir the reactionfor 1 hour at room temperature. Add an additional amount of methylene chloride (25 mL) and stir overnight. Dilute the reaction with ethyl acetate (100 mL), wash with water (100 mL) and dry the organic phase. Concentrate in vacuo and recrystallize the residue from ethyl acetate/hexane to yield the title compound (1.28 g, 81%); mp 234°-235° C.

후처리

  1. stirringstir overnight
  2. additionDilute
  3. washwash with water (100 mL)
  4. customdry the organic phase
  5. concentrationConcentrate in vacuo
  6. customrecrystallize the residue from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-06c69f9577954daa9e22a221be4b7289
출처 데이터셋
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05491153

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