Triethylamine → 4-(4-Chloro-phenoxymethyl)-benzylamine

HRID 2097353노트

반응식

HRID 2097353 반응식
[Cl:1][C:2]1[CH:19]=[CH:18][C:5]([O:6][CH2:7][C:8]2[CH:17]=[CH:16][C:11]([CH2:12][N:13]=[N+]=[N-])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.CCN(CC)CC.Cl[Sn]Cl>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH2:7][C:8]2[CH:17]=[CH:16][C:11]([CH2:12][NH2:13])=[CH:10][CH:9]=2)=[CH:18][CH:19]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 24479Stannous ChlorideHCID 231324374-(4-Chlorophenoxymethyl)-benzylazide

생성물 1

HCID 231324444-(4-Chloro-phenoxymethyl)-benzylamine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4-(4-Chloro-phenoxymethyl)-benzylazide (3.2 g, 11.7 mmol) was dissolved in MeOH (50 mL). NEt3 (11.35 mL, 81.9 mmol) and SnCl2×2H2O (5.28 g, 23.4 mmol) were added and the exothermic reaction was stirred under reflux. When boiling ceased the mixture was heated to reflux for additional 45 min. After cooling to r.t. the mixture was filtered and the filtrate was evaporated to dryness. The residue was dissolved in CH2Cl2 (300 mL) and this solution was washed with sat. aq. NaHCO3-solution (1×100 mL), dried over Na2SO4, filtered and evaporated to dryness to give the title compound, pure enough for further reaction.

후처리

  1. customthe exothermic reaction
  2. temperatureunder reflux
  3. temperaturewas heated
  4. temperatureto reflux for additional 45 min
  5. filtrationwas filtered
  6. customthe filtrate was evaporated to dryness
  7. dissolutionThe residue was dissolved in CH2Cl2 (300 mL)
  8. washthis solution was washed with sat. aq. NaHCO3-solution (1×100 mL)
  9. dry with materialdried over Na2SO4
  10. filtrationfiltered
  11. customevaporated to dryness

출처 및 근거

ORD 기록
ord-5dc0a59858f2425ea9ecd12ec1d888fd
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450348B2

반응 노트

불러오는 중…