(2-Chloro-4-nitrophenyl)(6,7,8,9-tetrahydro-5H-pyrido[3,2-b]azepin-5-yl)methanone → HCID 19438743, 화합물

HRID 1733960노트

반응식

HRID 1733960 반응식
[Cl:1][C:2]1[CH:20]=[C:19]([N+:21]([O-])=O)[CH:18]=[CH:17][C:3]=1[C:4]([N:6]1[CH2:12][CH2:11][CH2:10][CH2:9][C:8]2[N:13]=[CH:14][CH:15]=[CH:16][C:7]1=2)=[O:5].O.O.[Cl-]>CO>[NH2:21][C:19]1[CH:18]=[CH:17][C:3]([C:4]([N:6]2[CH2:12][CH2:11][CH2:10][CH2:9][C:8]3[N:13]=[CH:14][CH:15]=[CH:16][C:7]2=3)=[O:5])=[C:2]([Cl:1])[CH:20]=1

참가 물질

4

반응물 2

HCID 19699064(2-Chloro-4-nitrophenyl)(6,7,8,9-tetrahydro-5H-pyrido[3,2-b]azepin-5-yl)methanoneHCID 21226388Chloride dihydrate

생성물 1

HCID 19438743HCID 19438743, 화합물수율 85.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 3.31 g of 6,7,8,9-tetrahydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrido[3,2-b]azepine and 6.78 g of stannus chloride dihydrate (SnCl2.2H2O) in 200 ml of methanol is refluxed for 2 hours under argon. The solvent is removed under vacuum and 5 ml of saturated NaHCO3 solution and solid NaHCO3 added to bring the pH to 7. The mixture is extracted with ethyl acetate, the extract filtered through diatomaceous earth and the filtrate washed with saturated NaHCO3, H2O, brine and dried (Na2SO4). The filtrate is passed through a thin pad of hydrous magnesium silicate and the filtrate concentrated to dryness to give 2.58 g of an amorphous solid. Anal. Calc'd for C16H16ClN3O; C,59.9; H,5.7; N,13.1; C1, 11.1 Found: C,60.5; H,5.0; N,12.9; Cl,11.6.

후처리

  1. temperatureis refluxed for 2 hours under argon
  2. customThe solvent is removed under vacuum and 5 ml of saturated NaHCO3 solution and solid NaHCO3
  3. additionadded
  4. extractionThe mixture is extracted with ethyl acetate
  5. filtrationthe extract filtered through diatomaceous earth
  6. washthe filtrate washed with saturated NaHCO3, H2O, brine
  7. dry with materialdried (Na2SO4)
  8. concentrationthe filtrate concentrated to dryness

출처 및 근거

ORD 기록
ord-1cf4529766dd4497becb9e5e29b67966
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05532235

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