Water → 2-[4'-(3''-Hydroxypropoxy)phenyl]-6-iodoimidazo[1,2-a]pyridine

HRID 222229노트

반응식

HRID 222229 반응식
[O:1]([CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[N:20]=[C:21]3[CH:26]=[CH:25][C:24]([I:27])=[CH:23][N:22]3[CH:28]=2)=[CH:15][CH:14]=1)[Si](C(C)(C)C)(C)C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[Cl-].[NH4+].O>O1CCCC1.C(#N)C>[OH:1][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][C:16]([C:19]2[N:20]=[C:21]3[CH:26]=[CH:25][C:24]([I:27])=[CH:23][N:22]3[CH:28]=2)=[CH:17][CH:18]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 2724141Tetrabutylammonium FluorideHCID 671360922-[4'-(3''-t-Butyldimethylsiloxypropoxy)phenyl]-6-iodoimidazo[1,2-a]pyridine

생성물 1

HCID 247571022-[4'-(3''-Hydroxypropoxy)phenyl]-6-iodoimidazo[1,2-a]pyridine수율 87.3%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매2회

실험 절차

1.52 g (corresponding to 2.99 mmol) of 2-[4′-(3″-t-butyldimethylsiloxypropoxy)phenyl]-6-iodoimidazo[1,2-a]pyridine was dissolved in 5.0 mL of tetrahydrofuran, and 2.99 mL of a 1.0 mol/L tetrahydrofuran solution of tetrabutylammoniumfluoride was added thereto. After the reaction mixture was stirred at room temperature for 30 minutes, ammonium chloride solution was added followed by the addition of 10 mL of water and 5.0 mL of acetonitrile to filter precipitates. The filtered precipitates were washed with water and acetonitrile in this order, to obtain 1.03 g (corresponding to 2.61 mmol) of 2-[4′-(3″-hydroxypropoxy)phenyl]-6-iodoimidazo[1,2-a]pyridine (FIG. 10, Step 5).

후처리

  1. filtrationto filter
  2. customprecipitates
  3. customThe filtered precipitates
  4. washwere washed with water and acetonitrile in this order

출처 및 근거

ORD 기록
ord-82c5339c8ea94735b4965065c489ca69
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207189B2

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