Chlorotrimethylsilane → Methyl 4-(piperidin-4-yl)butanoate

HRID 1097288ノート

反応式

HRID 1097288 の反応式
[CH3:1][Si](Cl)(C)C.[NH:6]1[CH2:11][CH2:10][CH:9]([CH2:12][CH2:13][CH2:14][C:15]([OH:17])=[O:16])[CH2:8][CH2:7]1>CO>[CH3:1][O:16][C:15](=[O:17])[CH2:14][CH2:13][CH2:12][CH:9]1[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]1

参加物

4

反応物 2

HCID 6397ChlorotrimethylsilaneHCID 51677024-(Piperidin-4-yl)butanoic acid

生成物 1

HCID 21462751Methyl 4-(piperidin-4-yl)butanoate収率 100.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Trimethylsilyl chloride (9.2 ml, 72.46 mmol) was added to a solution of 4-piperidin-4-yl-butyric acid (1) (5.00 g, 24.15 mmol) dissolved in anhydrous methanol (100 mL). The resulting solution was stirred at room temperature for 48 hours, and concentrated under vacuum to complete dryness to give 2 (4.50 g, 97%) as a white solid, which was used directly in the next step without further purification: 1H NMR (300 MHz, CD3OD) δ 1.20-1.46 (m, 4H), 1.52-1.74 (m, 3H), 1.96 (d, 2H), 2.35 (t, 2H), 2.96 (t, 2H), 3.36 (t, 2H), 3.68 (s, 3H); ESI MS m/z 186 [C10H19NO2+H]+.

後処理

  1. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-5852ea171c3842fe9dcd0c6d841c6200
出典データセット
uspto-grants-2012_03
特許番号
US08143256B2

反応ノート

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