1,6-Dioxaspiro[2.5]octane → HCID 59255048, 화합물

HRID 1809345

반응식

HRID 1809345 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:3][CH2:2]1.[O:19]1[C:21]2([CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[CH2:20]1>CO>[OH:19][C:21]1([CH2:20][N:1]2[CH2:6][CH2:5][CH:4]([CH2:7][NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:3][CH2:2]2)[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1

참가 물질

4

반응물 2

HCID 1604391,6-Dioxaspiro[2.5]octaneHCID 14809798Benzyl (piperidin-4-ylmethyl)carbamate

생성물 1

HCID 59255048HCID 59255048, 화합물수율 49.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of benzyl (piperidin-4-ylmethyl)carbamate (7.77 g, 31.3 mmol, prepared according to Bose, D. Subhas et al., Tetrahedron Lett., 1990, 31, 6903) and 1,6-dioxaspiro[2.5]octane (4.29 g, 37.6 mmol, prepared according to Satyamurthy, Nagichettiar et al., Phosphorus Sulfur, 1984, 19, 113) in methanol (93 mL) was stirred at room temperature for 20 h. Then, the mixture was refluxed for 8 h. After cooling to room temperature, the solvent was removed in vacuo. The residue was chromatographed on a column of silica gel eluting with dichloromethane/methanol (v/v=20/1) to give 5.60 g (49%) of the title compound as colorless oil.

후처리

  1. temperatureThen, the mixture was refluxed for 8 h
  2. temperatureAfter cooling to room temperature
  3. customthe solvent was removed in vacuo
  4. customThe residue was chromatographed on a column of silica gel eluting with dichloromethane/methanol (v/v=20/1)

출처 및 근거

ORD 기록
ord-b2612b5d28144a91bc773913dc8ae9b8
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362038B2

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