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2,6-Diisopropylphenyl isocyanate → 1-(1-Benzenesulfonylcyclopentylmethyl)-3-(2,6-diisopropyl-phenyl)-urea

HRID 2061641
ノート
印刷プレビュー

反応式

HRID 2061641 の反応式
[N:1]([C:4]1[C:9]([CH:10]([CH3:12])[CH3:11])=[CH:8][CH:7]=[CH:6][C:5]=1[CH:13]([CH3:15])[CH3:14])=[C:2]=[O:3].[C:16]1([S:22]([C:25]2([CH2:30][NH2:31])[CH2:29][CH2:28][CH2:27][CH2:26]2)(=[O:24])=[O:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>ClCCl>[C:16]1([S:22]([C:25]2([CH2:30][NH:31][C:2]([NH:1][C:4]3[C:5]([CH:13]([CH3:15])[CH3:14])=[CH:6][CH:7]=[CH:8][C:9]=3[CH:10]([CH3:11])[CH3:12])=[O:3])[CH2:29][CH2:28][CH2:27][CH2:26]2)(=[O:23])=[O:24])[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 922592,6-Diisopropylphenyl isocyanateHCID 39871991HCID 39871991、化合物

生成物 1

HCID 252254811-(1-Benzenesulfonylcyclopentylmethyl)-3-(2,6-diisopropyl-phenyl)-urea収率 43.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In a tube, under nitrogen, 157 mg (0.77 mmol) of 2-isocyanato-1,3-diisopropylbenzene is added to a solution of 168 mg (0.7 mmol) of C-(1-benzenesulfonyl-cyclopentyl)-methylamine in 3.5 ml of dichloromethane. The reaction mixture is stirred at RT for 3 h. The solvent is evaporated with a nitrogen stream. The paste obtained is taken up in heptane (5 mL) for crystallization. The white powder obtained is chromatographed on silica gel (dichloromethane then dichloromethane/methanol, 98/2, v/v). The oil obtained is crystallized from heptane. After filtration and drying, 135 mg of 1-(1-benzenesulfonylcyclopentylmethyl)-3-(2,6-diisopropyl-phenyl)-urea is obtained in the form of a white powder (m.p.=124° C., Yield=44%).

後処理

  1. customThe solvent is evaporated with a nitrogen stream
  2. customThe paste obtained
  3. customis taken up in heptane (5 mL) for crystallization
  4. customThe white powder obtained
  5. customis chromatographed on silica gel (dichloromethane
  6. customThe oil obtained
  7. customis crystallized from heptane
  8. filtrationAfter filtration
  9. customdrying

出典と根拠

ORDレコード
ord-ab8873e8ca054dc393af7a5422ca4f5a
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08283378B2

反応ノート

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