Water → 2-Azaspiro[4.5]decane-3,8-dione

HRID 1190070노트

반응식

HRID 1190070 반응식
O1[C:5]2([CH2:15][CH2:14][C:8]3([CH2:12][C:11](=[O:13])[NH:10][CH2:9]3)[CH2:7][CH2:6]2)[O:4]CC1.O.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>CC(C)=O>[CH2:9]1[C:8]2([CH2:7][CH2:6][C:5](=[O:4])[CH2:15][CH2:14]2)[CH2:12][C:11](=[O:13])[NH:10]1

참가 물질

5

반응물 3

HCID 962WaterHCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 577954141,4-Dioxa-10-azadispiro[4.2.4^{8}.2^{5}]tetradecan-11-one

생성물 1

HCID 577955102-Azaspiro[4.5]decane-3,8-dione수율 58%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 1,4-dioxa-10-aza-dispiro[4.2.4.2]tetradecan-11-one (3.95 g, 18.7 mmol) in 160 mL of acetone was added 16 mL of water and pyridinium p-toluenesulfonate (1.41 g, 5.61 mmol). The resulting mixture was stirred at reflux for 20 h. Then, it was cooled and concentrated. The crude was purified by silica gel column chromatography using a 5% MeOH:EtOAc mixture as eluent to afford 2-aza-spiro[4.5]decane-3,8-dione (1.80 g, 58%) as a white solid.

후처리

  1. temperatureat reflux for 20 h
  2. temperatureThen, it was cooled
  3. concentrationconcentrated
  4. customThe crude was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-f82f3c339dda46e5b22afa40ce1f0765
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674118B2

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