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Potassium tert-butoxide → 2-Benzhydryl-5-oxa-2,8-diazaspiro[3.5]nonan-7-one

HRID 1689270
ノート
印刷プレビュー

反応式

HRID 1689270 の反応式
[CH:1]([N:14]1[CH2:17][C:16]([CH2:19][NH:20][C:21](=[O:24])[CH2:22]Cl)([OH:18])[CH2:15]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(C)([O-])C.[K+]>C1COCC1>[CH:1]([N:14]1[CH2:17][C:16]2([CH2:19][NH:20][C:21](=[O:24])[CH2:22][O:18]2)[CH2:15]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 23665647Potassium tert-butoxideHCID 57988954N-((1-Benzhydryl-3-hydroxyazetidin-3-yl)methyl)-2-chloroacetamide

生成物 1

HCID 579892642-Benzhydryl-5-oxa-2,8-diazaspiro[3.5]nonan-7-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
75 °C

実験手順

N-((1-Benzhydryl-3-hydroxyazetidin-3-yl)methyl)-2-chloroacetamide (example 33, step d) (2.6 g) in THF (50 mL) was added dropwise over 90 minutes to a vigorously stirred solution at 75° C. of potassium tert-butoxide (1M in tert-butanol, 15.08 mL) and THF (150 mL) under nitrogen. After the addition was complete the mixture was stirred at 75° C. for 10 minutes and then cooled to room temperature. The solvents were removed under reduced pressure and the residue was partitioned between ethyl acetate and brine. The organic layer was dried over sodium sulphate, filtered and the solvent removed under reduced pressure to afford the subtitled compound. Yield 2.05 g.

後処理

  1. additionAfter the addition
  2. temperaturecooled to room temperature
  3. customThe solvents were removed under reduced pressure
  4. customthe residue was partitioned between ethyl acetate and brine
  5. dry with materialThe organic layer was dried over sodium sulphate
  6. filtrationfiltered
  7. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-e8097f171b4047b8a992836f510946e3
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08148373B2

反応ノート

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