Methyl 2-[(2,6-dichlorobenzyl)amino]-3-(4-nitrophenyl)propanoate → HCID 11302630, 화합물

HRID 1869787

반응식

HRID 1869787 반응식
[Cl:1][C:2]1[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[C:3]=1[CH2:4][NH:5][CH:6]([CH2:11][C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-])=O)=[CH:14][CH:13]=1)[C:7]([O:9][CH3:10])=[O:8]>CC(O)=O>[NH2:18][C:15]1[CH:16]=[CH:17][C:12]([CH2:11][CH:6]([NH:5][CH2:4][C:3]2[C:21]([Cl:25])=[CH:22][CH:23]=[CH:24][C:2]=2[Cl:1])[C:7]([O:9][CH3:10])=[O:8])=[CH:13][CH:14]=1

참가 물질

3

반응물 1

HCID 11269078Methyl 2-[(2,6-dichlorobenzyl)amino]-3-(4-nitrophenyl)propanoate

생성물 1

HCID 11302630HCID 11302630, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To methyl 2-[(2,6-dichlorobenzyl)amino]-3-(4-nitrophenyl)propanoate 7a (8.2 g) solubilized in CH3COOH in an ultrasonic bath is added PtO2 hydrate (typical Pt content 79-84%) (0.02 g). A H2 pressure of 15 psi is then applied at RT and consumed after 5 min. An other H2 pressure of 10 psis is then applied at RT and consumed after 5-10 min. A H2 pressure of 10 psis is again applied at RT and a stabilization is observed after 5 min. The catalyst is filtered over celite under nitrogen and washed with CH3COOH. The solvent is evaporated. AcOEt (200 ml) is added to the residue and this organic phase is washed three times with saturated NaHCO3 (200 ml), dried over MgSO4 and evaporated. The residue is purified by silica gel chromatography using CH2Cl2/CH3OH/NH4OH cc (99.75/0.25/0.025) as eluent.

후처리

  1. customis then applied at RT
  2. customconsumed after 5 min
  3. customis then applied at RT
  4. customconsumed after 5-10 min
  5. customis again applied at RT
  6. filtrationThe catalyst is filtered over celite under nitrogen
  7. washwashed with CH3COOH
  8. customThe solvent is evaporated
  9. additionAcOEt (200 ml) is added to the residue
  10. washthis organic phase is washed three times with saturated NaHCO3 (200 ml)
  11. dry with materialdried over MgSO4
  12. customevaporated
  13. customThe residue is purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-66d3d69161b541ca8addcd5fcf33d69f
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07638630B2

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