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1-(2,2-Diphenylethyl)piperidin-4-one → 1-(2,2-Diphenylethyl)-4-methyl-4-piperidinol

HRID 1449062
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HRID 1449062 반응식
[C:1]1([CH:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:8][N:9]2[CH2:14][CH2:13][C:12](=[O:15])[CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:22][Mg]Br>O1CCCC1>[CH3:22][C:12]1([OH:15])[CH2:13][CH2:14][N:9]([CH2:8][CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:10][CH2:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 125156351-(2,2-Diphenylethyl)piperidin-4-oneHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 203750531-(2,2-Diphenylethyl)-4-methyl-4-piperidinol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 0.28 parts of 1-(2,2-diphenylethyl)-4-piperidinone in 5 parts by volume of tetrahydrofuran under nitrogen atmosphere is added 2 parts by volume of 3 M solution of methylmagnesium bromide. The resultant mixture is stirred for about 2.5 hours and then quenched with the careful addition of 5 parts by volume of 10% ammonium chloride. The mixture is left standing overnight, partitioned between water and ethyl acetate, and the organic layer separated. The organic layer is then dried with brine and magnesium sulfate, and concentrated to give 4-methyl-1-(2,2-diphenylethyl)-4-piperidinol, as yellow solid. This compound is represented by the following structural formula ##STR40##

후처리

  1. customquenched with the careful addition of 5 parts by volume of 10% ammonium chloride
  2. waitThe mixture is left
  3. custompartitioned between water and ethyl acetate
  4. customthe organic layer separated
  5. dry with materialThe organic layer is then dried with brine and magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-147ef1ad2cd4409f887076df6e895135
출처 데이터셋
uspto-grants-1980_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04188485

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