Carbon Tetrachloride → Ethyl 2-ethoxy-4-[N-(1-(2-piperidino-phenyl)-3-methyl-1-butyl)-aminocarbonylmethyl]benzoate

HRID 567586노트

반응식

HRID 567586 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH2:15][C:16]([OH:18])=O)[CH:7]=[CH:8][C:9]=1[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(N(CC)CC)C.C(Cl)(Cl)(Cl)Cl.[CH3:50][CH:51]([CH3:67])[CH2:52][CH:53]([NH2:66])[C:54]1[CH:59]=[CH:58][CH:57]=[CH:56][C:55]=1[N:60]1[CH2:65][CH2:64][CH2:63][CH2:62][CH2:61]1>C(#N)C>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH2:15][C:16]([NH:66][CH:53]([C:54]2[CH:59]=[CH:58][CH:57]=[CH:56][C:55]=2[N:60]2[CH2:61][CH2:62][CH2:63][CH2:64][CH2:65]2)[CH2:52][CH:51]([CH3:67])[CH3:50])=[O:18])[CH:7]=[CH:8][C:9]=1[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH3:2]

참가 물질

7

반응물 5

HCID 5943Carbon TetrachlorideHCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 101312123-Ethoxy-4-ethoxycarbonylphenylacetic acidHCID 104220523-Methyl-1-(2-piperidino-phenyl)-1-butylamine

생성물 1

HCID 13729227Ethyl 2-ethoxy-4-[N-(1-(2-piperidino-phenyl)-3-methyl-1-butyl)-aminocarbonylmethyl]benzoate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

3 g (11.9 mmols) of 3-ethoxy-4-ethoxycarbonylphenylacetic acid, 3.7 g (14.3 mmols) of triphenylphosphine, 3.3 ml (23.8 mmols) of triethylamine and 1.15 ml (11.9 mmols) of carbon tetrachloride were added successively to a solution of 2.9 g (11.9 mmols) of 3-methyl-1-(2-piperidino-phenyl)-1-butylamine in 29 of acetonitrile. The mixture was then stirred for 15 hours at room temperature, the solvent was removed in vacuo, and the residue was taken up in a mixture of ethyl acetate and water. The organic phase was dried over sodium sulfate, filtered and concentrated by evaporation in vacuo. The evaporation residue was purified by column chromatography on silaca gel (toluene/acetone=10/1).

후처리

  1. customthe solvent was removed in vacuo
  2. additionthe residue was taken up in a mixture of ethyl acetate and water
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated by evaporation in vacuo
  6. customThe evaporation residue was purified by column chromatography on silaca gel (toluene/acetone=10/1)

출처 및 근거

ORD 기록
ord-cd52593611594f5ba3345129da385455
출처 데이터셋
uspto-grants-2001_01
특허 번호
USRE037035E1

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