1-(4-Chlorobenzyl)-7-cyclohexyl-1,7-diazaspiro[4.4]nonane-3,6-dione → 1-(4-Chlorobenzyl)-7-cyclohexyl-3-hydroxy-3-methyl-1,7-diazaspiro[4.4]nonan-6-one

HRID 1672395

반응식

HRID 1672395 반응식
[CH3:1]C(=C)C[Mg]Cl.[Cl:7][C:8]1[CH:31]=[CH:30][C:11]([CH2:12][N:13]2[C:17]3([CH2:21][CH2:20][N:19]([CH:22]4[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]4)[C:18]3=[O:28])[CH2:16][C:15](=[O:29])[CH2:14]2)=[CH:10][CH:9]=1>C1COCC1>[Cl:7][C:8]1[CH:9]=[CH:10][C:11]([CH2:12][N:13]2[C:17]3([CH2:21][CH2:20][N:19]([CH:22]4[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]4)[C:18]3=[O:28])[CH2:16][C:15]([OH:29])([CH3:1])[CH2:14]2)=[CH:30][CH:31]=1

참가 물질

4

반응물 2

HCID 673556101-(4-Chlorobenzyl)-7-cyclohexyl-1,7-diazaspiro[4.4]nonane-3,6-dioneHCID 178448200HCID 178448200, 화합물

생성물 1

HCID 673550741-(4-Chlorobenzyl)-7-cyclohexyl-3-hydroxy-3-methyl-1,7-diazaspiro[4.4]nonan-6-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
50 °C

실험 절차

2-Methylallylmagnesium chloride in THF (3.0 M, 0.074 mL) was added to a solution of 1-(4-chlorobenzyl)-7-cyclohexyl-1,7-diazaspiro[4.4]nonane-3,6-dione (0.040 g, 0.00011 mol) in THF (1.0 mL, 0.012 mol) and the resulting mixture was stirred at 50° C. for 1 h. The reaction mixture was then allowed to cool to RT and was then quenched by the addition of saturated NH4Cl. The crude reaction mixture was purified by prep. HPLC to afford the desired product. LC/MS: 377.2 (M+1H)+.

후처리

  1. temperatureto cool to RT
  2. customwas then quenched by the addition of saturated NH4Cl
  3. customThe crude reaction mixture
  4. customwas purified by prep

출처 및 근거

ORD 기록
ord-80b753a146c34d1dbd5a5a21ce81fd5c
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998959B2

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