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Phosgene → HCID 15053365, 화합물

HRID 2081380
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HRID 2081380 반응식
[C:1]([Cl:4])(Cl)=[O:2].C(=O)([O-])[O-].[K+].[K+].[Br:11][C:12]1[CH:13]=[C:14]([CH:33]=[CH:34][CH:35]=1)[O:15][CH:16]1[CH2:19][N:18](C(C2C=CC=CC=2)C2C=CC=CC=2)[CH2:17]1>C(Cl)Cl>[Br:11][C:12]1[CH:13]=[C:14]([CH:33]=[CH:34][CH:35]=1)[O:15][CH:16]1[CH2:19][N:18]([C:1]([Cl:4])=[O:2])[CH2:17]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6371PhosgeneHCID 11430Potassium CarbonateHCID 15053370HCID 15053370, 화합물

생성물 1

HCID 15053365HCID 15053365, 화합물수율 175.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 22.7 g (0.23 mole) of phosgene in 200 ml of methylene chloride was treated with 29 g (0.23 mole) of potassium carbonate, stirred for 30 min, then 75.4 g (0.19 mole) of 3-(3-bromophenoxy)-1-diphenylmethylazetidine in 150 ml of methylene chloride was added dropwise. After stirring for 5 hr, the inorganic salts were removed by filtration and the filtrate was washed with water to destroy excess phosgene. Concentration (after drying) in vacuo yielded 96.85 g of oily residue. Trituration of the residue with isopropyl ether yielded 42 g of crude tan-gray product. A sample for analysis was recrystallized from isopropyl ether, m.p. 87°-88° C.

후처리

  1. stirringAfter stirring for 5 hr
  2. customthe inorganic salts were removed by filtration
  3. washthe filtrate was washed with water
  4. customto destroy excess phosgene
  5. concentrationConcentration (after drying) in vacuo

출처 및 근거

ORD 기록
ord-5804d00dd56e4dff8dd2f94c46209ed8
출처 데이터셋
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05183902

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