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Methane, dichloromethoxy- → HCID 18921503, 화합물

HRID 1654959
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HRID 1654959 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[Cl:5][C:6]1[CH:11]=[CH:10][C:9]([S:12]([NH:15][CH2:16][CH:17]2[CH2:25][C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH2:18]2)(=[O:14])=[O:13])=[CH:8][CH:7]=1.Cl[CH:27]([O:29]C)Cl>C(Cl)Cl>[CH:27]([C:21]1[CH:20]=[C:19]2[C:24](=[CH:23][CH:22]=1)[CH2:25][CH:17]([CH2:16][NH:15][S:12]([C:9]1[CH:8]=[CH:7][C:6]([Cl:5])=[CH:11][CH:10]=1)(=[O:14])=[O:13])[CH2:18]2)=[O:29]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 21004Methane, dichloromethoxy-HCID 6451240Aluminum(III) ChlorideHCID 189215132-[(4-Chlorophenyl)sulfonylaminomethyl)indan

생성물 1

HCID 18921503HCID 18921503, 화합물수율 22%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
-20 °C

실험 절차

5.33 g (40.0 mmol) of anhydrous aluminum chloride was suspended in 20 ml of methylenechloride and added with 1.61 g (5.00 mmol) of 2-[(4-chlorophenyl)sulfonylaminomethyl]indan, followed by cooling at -20° C. 10 ml of methylene chloride containing as dissolved 0.68 ml (7.5 mmol) of dichloromethylmethylether was slowly added dropwise thereto, followed by stirring for 1 hour at the same temperature. The reaction solution was poured into ice-water and stirred for 1 hour. Thereafter, the organic phase was collected, washed, dried, and the solvent was removed. The residue was purified by silica gel column chromatography (chloroform), followed by recrystallizing from a solvent mixture of ethylacetate and hexane to obtain 375 mg of colorless crystals. Yield: 22%

후처리

  1. additionwas slowly added dropwise
  2. stirringstirred for 1 hour
  3. customThereafter, the organic phase was collected
  4. washwashed
  5. customdried
  6. customthe solvent was removed
  7. customThe residue was purified by silica gel column chromatography (chloroform)
  8. customby recrystallizing from a solvent mixture of ethylacetate and hexane

출처 및 근거

ORD 기록
ord-3a9d871d6eff468c92fee0e2b12d8ce2
출처 데이터셋
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05409956

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