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

HRID 1869787

反応式

HRID 1869787 の反応式
[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

参加物

3

反応物 1

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

生成物 1

HCID 11302630HCID 11302630、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-66d3d69161b541ca8addcd5fcf33d69f
出典データセット
uspto-grants-2009_12
特許番号
US07638630B2

関連ノート

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