(+)-trans-1-(3,4-Dichlorobenzamido)-2-acetoxy-7-nitrotetraline → (+)-trans-1-(3,4-Dichlorobenzamido)-2-acetoxy-7-aminotetraline

HRID 1937362노트

반응식

HRID 1937362 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][C:27]=1[Cl:28])[C:5]([NH:7][C@@H:8]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([N+:18]([O-])=O)[CH:16]=2)[CH2:11][CH2:10][C@H:9]1[O:21][C:22](=[O:24])[CH3:23])=[O:6]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][C:27]=1[Cl:28])[C:5]([NH:7][C@@H:8]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([NH2:18])[CH:16]=2)[CH2:11][CH2:10][C@H:9]1[O:21][C:22](=[O:24])[CH3:23])=[O:6]

참가 물질

3

반응물 1

HCID 21338526(+)-trans-1-(3,4-Dichlorobenzamido)-2-acetoxy-7-nitrotetraline

생성물 1

HCID 12042344(+)-trans-1-(3,4-Dichlorobenzamido)-2-acetoxy-7-aminotetraline수율 107.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 114 (1.9 g) in DMF (100 mL) was treated with SnCl2-2H2O (4 g). After 4 h, additional SnC2-2H2O (1 g) was added three times over three days. The solvent was then evaporated, the residue suspended in H2O-EtOAc, the mixture neutralized with 5N NaOH, and the mixture filtered. The organics were separated, washed with brine, dried, and the solvent evaporated to give a brown foam (1.9 g).

후처리

  1. customThe solvent was then evaporated
  2. filtrationthe mixture filtered
  3. customThe organics were separated
  4. washwashed with brine
  5. customdried
  6. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-2f7befe43d9841beadc11965c19e92ec
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06395735B2

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