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Water → HCID 19771132, 화합물

HRID 1589870
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HRID 1589870 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][C:10]([NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[O:19][CH3:20])=[O:11].[OH-].[Na+].Cl[O-].[Na+].O>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C(Cl)Cl.CO>[CH3:20][O:19][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=1[N:12]1[C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[C:4]=2[NH:9][C:10]1=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 295258N,N'-bis(2-methoxyphenyl)ureaHCID 23665760Sodium Hypochlorite

생성물 1

HCID 19771132HCID 19771132, 화합물

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매
HCID 21226129
Dichloromethane methanol
용매

실험 절차

A mixture of N,N'-di-(2-methoxyphenyl)-urea (6.81 g, 25 mmol) and tetra-n-butyl-ammoniumbromide (0.4 g, 1.3 mmol) in methylene chloride/methanol (1:1 , 200 ml) was at room temperature under vigorous stirring added a solution of sodium hydroxide (2 g in 10 ml water) followed by a solution of sodiumhypochlorite(55 ml, Aldrich). The mixture was stirred for 4 hours and 30 ml water was added The organic phase was washed with 10 ml 1M hydrogen chloride sol., dried and concentrated in vacuo. Upon trituration with diethyl ether dark grey crystals separated The crude product was recrystallized twice, first from ethanol and then from ethyl acetate yielding the title compound as white crystals, M.p. 246°-247° C.

후처리

  1. customwas at room temperature
  2. stirringThe mixture was stirred for 4 hours
  3. washwas washed with 10 ml 1M hydrogen chloride sol.
  4. customdried
  5. concentrationconcentrated in vacuo
  6. customUpon trituration with diethyl ether dark grey crystals separated The crude product
  7. customwas recrystallized twice, first from ethanol

출처 및 근거

ORD 기록
ord-7dcec4063adf42988fb08d184ad19693
출처 데이터셋
uspto-grants-1993_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05200422

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