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Water → HCID 19771132、化合物

HRID 1589870
ノート
印刷プレビュー

反応式

HRID 1589870 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

HCID 19771132HCID 19771132、化合物

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒
HCID 21226129
Dichloromethane methanol
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7dcec4063adf42988fb08d184ad19693
出典データセット
uspto-grants-1993_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05200422

反応ノート

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