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2-(Phenylmethanesulfinyl)aniline → HCID 13672816, 화합물

HRID 1732012
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HRID 1732012 반응식
[CH2:1]([S:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1N)=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N([O-])=O.[Na+]>OS(O)(=O)=O.O>[CH:14]1[C:15]2[C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[CH2:1][S:8](=[O:9])[C:10]=2[CH:11]=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 136728152-(Phenylmethanesulfinyl)anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 13672816HCID 13672816, 화합물수율 72.9%

시약·촉매·용매 2

HCID 962Water용매2회HCID 1118Sulfuric Acid용매

실험 절차

To a stirred suspension of benzyl-(2-aminophenyl)-sulfoxide (1.9 g; 0.008 mol) in 30 ml of 11% H2SO4 was added a solution of sodium nitrite (0.78 g; 0.011 mol) in 20 ml of water at about 0° C. After 1 hour at 0° C. to the yellow solution was quickly added a solution of cupric nitrate trihydrate (34.2 g; 0.140 mol) in 75 ml of water and cuprous oxide (1.33 g; 0.009 mol). The solution was allowed to warm to room temperature and stirred for further 5 hours. The solid was filtered and treated with hot ethyl acetate. The solution was dried over sodium sulfate concentrated and the residue was crystallized from ethyl acetate/pentane (1:4) to give 6H-dibenzo[b,d]thiopyran-5-oxide (1.25 g; yield 71%); m.p. 97°-100° C. By proceeding analogously the following compounds were obtained:

후처리

  1. filtrationThe solid was filtered
  2. additiontreated with hot ethyl acetate
  3. dry with materialThe solution was dried over sodium sulfate
  4. concentrationconcentrated
  5. customthe residue was crystallized from ethyl acetate/pentane (1:4)

출처 및 근거

ORD 기록
ord-23bb45b8257f4da68003739bb160d46e
출처 데이터셋
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04624949

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