Water → 2-(4-(6-Iodoimidazo(1,2-a)pyridin-2-yl)phenoxy)ethanol

HRID 222220노트

반응식

HRID 222220 반응식
[O:1]([CH2:19][CH2:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]2[N:29]=[C:30]3[CH:35]=[CH:34][C:33]([I:36])=[CH:32][N:31]3[CH:37]=2)=[CH:24][CH:23]=1)[Si](C(C)(C)C)(C1C=CC=CC=1)C1C=CC=CC=1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[Cl-].[NH4+].O>O1CCCC1.C(#N)C>[OH:1][CH2:19][CH2:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]2[N:29]=[C:30]3[CH:35]=[CH:34][C:33]([I:36])=[CH:32][N:31]3[CH:37]=2)=[CH:24][CH:23]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 2724141Tetrabutylammonium FluorideHCID 671360362-[4'-(2''-t-Butyldiphenylsiloxyethoxy)phenyl]-6-iodoimidazo[1,2-a]pyridine

생성물 1

HCID 247570132-(4-(6-Iodoimidazo(1,2-a)pyridin-2-yl)phenoxy)ethanol수율 100%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매2회

실험 절차

368 mg (corresponding to 0.595 mmol) of 2-[4′-(2″-t-butyldiphenylsiloxyethoxy)phenyl]-6-iodoimidazo[1,2-a]pyridine was dissolved in 1.0 mL of tetrahydrofuran (THF), and 0.70 mL of a 1.0 mol/L solution in tetrahydrofuran of tetrabutylammoniumfluoride (TBAF) was added thereto. After the reaction mixture was stirred at room temperature for 2 hours, ammonium chloride aqueous solution was added, followed by addition of 5.0 mL of water and 2.0 mL of acetonitrile. Then precipitates were filtered. The filtered precipitates were washed with water and acetonitrile in this order, to obtain 226 mg (corresponding to 0.595 mmol) of 2-[4′-(2″-hydroxyethoxy)phenyl]-6-iodoimidazo[1,2-a]pyridine (FIG. 1, Step 5).

후처리

  1. customThen precipitates
  2. filtrationwere filtered
  3. customThe filtered precipitates
  4. washwere washed with water and acetonitrile in this order

출처 및 근거

ORD 기록
ord-a437f678a82843479207aac0305d3e4d
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207189B2

반응 노트

불러오는 중…