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

HRID 1857599

반응식

HRID 1857599 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-99c82563287f4567a78407e5a3ea2560
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147116

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