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Benzyl Bromide → 6-Benzyl-8,8-dimethyl-6,9-diaza-spiro[4.5]decan-10-one

HRID 2360712
ノート
印刷プレビュー

反応式

HRID 2360712 の反応式
[CH3:1][C:2]1([CH3:13])[NH:11][C:10](=[O:12])[C:5]2([CH2:9][CH2:8][CH2:7][CH2:6]2)[NH:4][CH2:3]1.[CH2:14](Br)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[CH2:14]([N:4]1[CH2:3][C:2]([CH3:13])([CH3:1])[NH:11][C:10](=[O:12])[C:5]21[CH2:9][CH2:8][CH2:7][CH2:6]2)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 81531DiisopropylethylamineHCID 86680334HCID 86680334、化合物

生成物 1

HCID 866803356-Benzyl-8,8-dimethyl-6,9-diaza-spiro[4.5]decan-10-one収率 96%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 6.72 g of 8,8-dimethyl-6,9-diaza-spiro[4.5]decan-10-one in 35 ml of DMF were added 4.8 ml of benzyl bromide and 6.9 ml of Hünig's base. The reaction was stirred at r.t overnight. The precipitated product was isolated by suction and washed with DMF and EtOAc. The filtrate was concentrated and the resulting residue was dissolved in EtOAc, washed with water, dried over Na2SO4, filtered and concentrated to yield a second fraction of the product. 9.62 g (96%) of the title compound were obtained.

後処理

  1. customThe precipitated product was isolated by suction
  2. washwashed with DMF and EtOAc
  3. concentrationThe filtrate was concentrated
  4. dissolutionthe resulting residue was dissolved in EtOAc
  5. washwashed with water
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto yield a second fraction of the product

出典と根拠

ORDレコード
ord-cc2af8a3689349c58515bf4db50d65f7
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08686150B2

反応ノート

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