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

HRID 2302078노트

반응식

HRID 2302078 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 SnCl22H2O (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. additionadditional SnCl22H2O (1 g) was added three times over three days
  2. customThe solvent was then evaporated
  3. filtrationthe mixture filtered
  4. customorganics were separated
  5. washwashed with brine
  6. customdried
  7. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-e02eb76ba2bd40e3bcba89907a5377cc
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06429317B1

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