4,4-Diaminodiphenylmethane → 1-(4-Nitrophenyl)-3-[4-[[4-[(4-nitrophenyl)carbamothioylamino]phenyl]methyl]phenyl]thiourea

HRID 619406

反応式

HRID 619406 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]=[C:11]=[S:12])=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH:13]1[C:18]([CH2:19][C:20]2[CH:25]=[CH:24][C:23]([NH2:26])=[CH:22][CH:21]=2)=[CH:17][CH:16]=[C:15]([NH2:27])[CH:14]=1>O1CCOCC1>[CH2:19]([C:20]1[CH:25]=[CH:24][C:23]([NH:26][C:11]([NH:10][C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=2)=[S:12])=[CH:22][CH:21]=1)[C:18]1[CH:13]=[CH:14][C:15]([NH:27][C:11]([NH:10][C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=2)=[S:12])=[CH:16][CH:17]=1

参加物

4

反応物 2

HCID 75774,4-DiaminodiphenylmethaneHCID 75044Benzene, 1-isothiocyanato-4-nitro-

生成物 1

HCID 64813501-(4-Nitrophenyl)-3-[4-[[4-[(4-nitrophenyl)carbamothioylamino]phenyl]methyl]phenyl]thiourea

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

A solution of 4-nitrophenyl isothiocyanate (0.45 g, 2.52 mmol) in dioxane (25 mL) is slowly added, with magnetic stirring, to a solution of 4,4'-diaminodiphenyl methane (0.25 g, 1.26 mmol) in dioxane (10 mL). After 24 hours of stirring at room temperature, the solvent is removed by vacuum evaporation. The solid obtained is washed with n-hexane (3×25 mL) and isopropanol (3×10 mL). Next, the solid is dissolved in ethyl acetate (50 mL) and washed with water (3×25 mL). The organic phase is dried with sodium sulfate. The solvent is removed by vacuum evaporation. The titled compound is obtained as a yellow powder. mp: 115° C.

後処理

  1. customthe solvent is removed by vacuum evaporation
  2. customThe solid obtained
  3. washis washed with n-hexane (3×25 mL) and isopropanol (3×10 mL)
  4. dissolutionNext, the solid is dissolved in ethyl acetate (50 mL)
  5. washwashed with water (3×25 mL)
  6. dry with materialThe organic phase is dried with sodium sulfate
  7. customThe solvent is removed by vacuum evaporation

出典と根拠

ORDレコード
ord-1dfb514b41ed46ddbf8d4d4c23a2d751
出典データセット
uspto-grants-1999_09
特許番号
US05958983

関連ノート

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