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

HRID 1890202ノート

反応式

HRID 1890202 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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. 2-10, Step 5).

後処理

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

出典と根拠

ORDレコード
ord-aff00e9753ba4e44b2f816bee3fc7864
出典データセット
uspto-grants-2013_08
特許番号
US08506930B2

反応ノート

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