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tert-butyl N-methyl-N-(2-oxoethyl)carbamate → tert-Butyl 2-(4-(dimethylamino)-4-phenylpiperidin-1-yl)ethyl(methyl)carbamate

HRID 1500316
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HRID 1500316 반응식
[CH3:1][N:2]([CH3:15])[C:3]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.[CH3:16][N:17]([CH2:25][CH:26]=O)[C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21].C(B)#N.[Na]>CO.C(O)(=O)C.CO.C(Cl)(Cl)Cl>[CH3:1][N:2]([CH3:15])[C:3]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:4][CH2:5][N:6]([CH2:26][CH2:25][N:17]([CH3:16])[C:18](=[O:24])[O:19][C:20]([CH3:22])([CH3:21])[CH3:23])[CH2:7][CH2:8]1
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참가 물질

7

반응물 3

HCID 10725881tert-butyl N-methyl-N-(2-oxoethyl)carbamateHCID 57831258N,N-dimethyl-4-phenylpiperidin-4-amineHCID 101953985CID 1019539852회

생성물 1

HCID 68408263tert-Butyl 2-(4-(dimethylamino)-4-phenylpiperidin-1-yl)ethyl(methyl)carbamate수율 64.6%

시약·촉매·용매 3

HCID 176Acetic Acid용매2회
HCID 887
Methanol
용매
HCID 21584188Chloroform methanol용매

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온도
0 °C

실험 절차

7 g (1 eq) N,N-dimethyl-4-phenylpiperidin-4-amine were added in portions to a solution of 6.5 g (1.5 eq) tert-butyl methyl(2-oxoethyl)carbamate in 60 ml methanol. This reaction mixture was cooled to 0° C., 3.97 g (2.5 eq) sodium cyanoboron hydride were added in portions and then the mixture was stirred for 10 min at room temperature. The reaction mixture obtained was adjusted to a pH of ˜5 with acetic acid and stirred for 12 h at room temperature. The reaction course was monitored by thin-layer chromatography (20% MeOH/CHCl3). As the conversion was still not complete, 1.5 g sodium cyanoboron hydride and acetic acid were added and the reaction mixture was stirred for a further 30 to 45 min. Once the conversion was complete, the methanol was distilled off, 100 ml saturated NaHCO3 solution were added and the mixture obtained was extracted with chloroform (2×200 ml) and the combined organic phases were dried over Na2SO4. Following removal of the solvent under reduced pressure, the residue was purified by column chromatography (silica gel; 5% MeOH/CHCl3). 8 g (64%) of product were obtained in the form of an oil.

후처리

  1. customThe reaction mixture obtained
  2. stirringstirred for 12 h at room temperature
  3. stirringthe reaction mixture was stirred for a further 30 to 45 min
  4. distillationthe methanol was distilled off
  5. addition100 ml saturated NaHCO3 solution were added
  6. customthe mixture obtained
  7. extractionwas extracted with chloroform (2×200 ml)
  8. dry with materialthe combined organic phases were dried over Na2SO4
  9. customremoval of the solvent under reduced pressure
  10. customthe residue was purified by column chromatography (silica gel; 5% MeOH/CHCl3)

출처 및 근거

ORD 기록
ord-a0734f17f27c4df0b298e3c853566bff
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09206156B2

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