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

HRID 1097288노트

반응식

HRID 1097288 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 21462751Methyl 4-(piperidin-4-yl)butanoate수율 100.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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]+.

후처리

  1. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-5852ea171c3842fe9dcd0c6d841c6200
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143256B2

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