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Sodium Iodide → HCID 70873537, 화합물

HRID 2172224
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HRID 2172224 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[NH:15][CH2:14][CH2:13][CH2:12]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[CH2:20][CH2:21][CH2:22][O:23][C:24]1[CH:29]=[CH:28][C:27]([O:30][C:31]([F:34])([F:33])[F:32])=[CH:26][CH:25]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN1C(=O)CCC1.O>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]([CH2:20][CH2:21][CH2:22][O:23][C:24]1[CH:29]=[CH:28][C:27]([O:30][C:31]([F:32])([F:33])[F:34])=[CH:26][CH:25]=1)[CH2:14][CH2:13][CH2:12]2)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 2233929075893-80-0HCID 86709383HCID 86709383, 화합물

생성물 1

HCID 70873537HCID 70873537, 화합물수율 93.1%

시약·촉매·용매 2

HCID 962Water용매
HCID 13387
N-methyl-2-pyrrolidone
용매

실험 절차

6-Benzyloxy-1,2,3,4-tetrahydro-quinoline (1.20 g, 5 mmol), 1-(3-chloropropoxy)-4-trifluoromethoxybenzene (1.42 g, 5.58 mmol), potassium carbonate (1.04 g, 7.5 mmol) and sodium iodide (0.90 g, 6 mmol) were heated and stirred at 90° C. in NMP (10 ml) overnight. Water was added thereto, followed by extraction with ethyl acetate. The organic layer was washed with water and dried over sodium sulfate. The result was concentrated and purified by silica gel column chromatography (hexane:ethyl acetate=75:25) to afford the title compound as a yellow oil (2.13 g, 93%).

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationThe result was concentrated
  5. custompurified by silica gel column chromatography (hexane:ethyl acetate=75:25)

출처 및 근거

ORD 기록
ord-bbaa5ceeebbb4b8b8e5055725557e5b8
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09051333B2

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