1,6-Dioxaspiro[2.5]octane → HCID 59255048、化合物

HRID 502899

反応式

HRID 502899 の反応式
[CH2:1]([O:8][C:9](=[O:18])[NH:10][CH2:11][CH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[O:19]1[C:21]2([CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[CH2:20]1>CO>[CH2:1]([O:8][C:9](=[O:18])[NH:10][CH2:11][CH:12]1[CH2:13][CH2:14][N:15]([CH2:20][C:21]2([OH:19])[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[CH2:16][CH2:17]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

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

生成物 1

HCID 59255048HCID 59255048、化合物収率 49.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of benzyl(piperidin-4-ylmethyl)carbamate (7.77 g, 31.3 mmol, Bose, D. Subhas et al., Tetrahedron Lett., 1990, 31, 6903) and 1,6-dioxaspiro[2.5]octane (4.29 g, 37.6 mmol, 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 methanol/dichloromethane (1:20) to give 5.60 g (49%) of the title compound as a colorless oil.

後処理

  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 methanol/dichloromethane (1:20)

出典と根拠

ORDレコード
ord-d4f72b04d6c74d59b3097ea0e8ff5696
出典データセット
uspto-grants-2010_08
特許番号
US07776885B2

関連ノート

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