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

HRID 2279180
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HRID 2279180 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 81531DiisopropylethylamineHCID 86680334HCID 86680334, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-35f5e1d0fba84574b4cc4ab171f417fe
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09133181B2

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