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3-Methylbutanal → HCID 18441751, 화합물

HRID 458147
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HRID 458147 반응식
[CH2:1]([N:8]1[CH2:18][CH2:17][C:11]2([NH:15][CH2:14][NH:13][C:12]2=[O:16])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:19](=O)[CH2:20][CH:21]([CH3:23])[CH3:22].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCCl>[CH2:1]([N:8]1[CH2:9][CH2:10][C:11]2([N:15]([CH2:19][CH2:20][CH:21]([CH3:23])[CH3:22])[CH2:14][NH:13][C:12]2=[O:16])[CH2:17][CH2:18]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 115523-MethylbutanalHCID 5049666Sodium triacetoxyborohydrideHCID 105383388-benzyl-1,3,8-triazaspiro[4.5]decan-4-one

생성물 1

HCID 18441751HCID 18441751, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

To a solution of 100 mg (0.408 mmol) 8-benzyl-1,3,8-triaza-spiro[4,5]decan-4-one (m.p. 164–166° C.) and 0.062 ml (49.2 mg, 0.571 mmol) isovaleraldehyde in 3 ml 1,2-dichloroethane were added 130 mg (0.611 mmol) sodium triacetoxyborohydride and the mixture stirred at ambient temperature for 16 h. Then the reaction mixture was quenched with 10 ml saturated aqueous NaHCO3-solution and extracted with dichloromethane. The organic extracts were washed with brine, dried over Na2SO4, filtered and evaporated: 128 mg 8-benzyl-1-(3-methyl-butyl)-1,3,8-triaza-spiro[4.5]decan-4-one as colorless crystals: m.p. 139–140° C., MS (ISP): 316.4 MH+.

후처리

  1. customThen the reaction mixture was quenched with 10 ml saturated aqueous NaHCO3-solution
  2. extractionextracted with dichloromethane
  3. washThe organic extracts were washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-1a26af7f9bbd4c739739dc46a7a50279
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07189850B2

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