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Ammonium Acetate → HCID 14745920, 화합물

HRID 1085236
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HRID 1085236 반응식
[Cl:1]/[C:2](/[C:9]([O:11][CH3:12])=[O:10])=[C:3](\Cl)/[C:4]([O:6][CH3:7])=[O:5].C([O-])(=O)C.[NH4+:17]>CN(C)C=O>[NH2:17]/[C:3](/[C:4]([O:6][CH3:7])=[O:5])=[C:2](\[Cl:1])/[C:9]([O:11][CH3:12])=[O:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 3034513Dimethyl 2,3-dichloromaleate

생성물 1

HCID 14745920HCID 14745920, 화합물수율 83%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

53.25 g (0.25 mol) of dimethyl dichloromaleate were dissolved in 100 ml of dimethylformamide, and 48.16 g (0.625 mol) of ammonium acetate were added. The mixture was rapidly heated to 120° C. and stirred at 110° C. to 120° C. for one hour. The solvent was subsequently removed by distillation, the residue was taken up in methylene chloride, and the solution was washed with water. The methylene chloride was removed by distillation on an evaporator, and, after recrystallization, 40 g (83% yield) of dimethyl aminochloromaleate were obtained in the form of yellowish, cubic crystals (m.p. 96°-98° C.)

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후처리

  1. customThe solvent was subsequently removed by distillation
  2. washthe solution was washed with water
  3. customThe methylene chloride was removed by distillation on an evaporator
  4. customafter recrystallization

출처 및 근거

ORD 기록
ord-c664d1829b564d459aaa9b4042638d0d
출처 데이터셋
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05008392

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