4-Piperidinemethanol → HCID 52234807、化合物

HRID 2407677ノート

反応式

HRID 2407677 の反応式
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[C:15]1([C:21]2[CH:25]=[C:24]([CH:26]=O)[O:23][N:22]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[NH:28]1[CH2:33][CH2:32][CH:31]([CH2:34][OH:35])[CH2:30][CH2:29]1>ClCCl>[C:15]1([C:21]2[CH:25]=[C:24]([CH2:26][N:28]3[CH2:33][CH2:32][CH:31]([CH2:34][OH:35])[CH2:30][CH2:29]3)[O:23][N:22]=2)[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

5

反応物 3

HCID 4207714-PiperidinemethanolHCID 5049666Sodium triacetoxyborohydrideHCID 113672673-Phenyl-1,2-oxazole-5-carbaldehyde

生成物 1

HCID 52234807HCID 52234807、化合物収率 102.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Sodium triacetoxyborohydride (12.2 g) was added portionwise to a room temperature mixture of the compound prepared in Example 7 (5.00 g) and piperidin-4-ylmethanol (4.99 g) in dichloromethane (150 mL). The reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with dichloromethane and washed sequentially with a saturated aqueous sodium bicarbonate solution and brine. The organics were dried over anhydrous magnesium sulfate and concentrated to obtain the crude title compound (8.05 g), which was used without further purification having the following physical data.

後処理

  1. washwashed sequentially with a saturated aqueous sodium bicarbonate solution and brine
  2. dry with materialThe organics were dried over anhydrous magnesium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-ac4271aac7e448568fa0134caf35d304
出典データセット
uspto-grants-2014_08
特許番号
US08809538B2

反応ノート

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