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2-amino-3,6-dichloroPhenol → 2-Chloromethyl-4,7-dichlorobenzoxazole

HRID 1033032
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HRID 1033032 반응식
[NH2:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[C:4]([Cl:9])[C:3]=1[OH:10].[ClH:11].ClN=CC(O[CH2:18][CH3:19])=O>C(Cl)Cl>[Cl:11][CH2:18][C:19]1[O:10][C:3]2[C:4]([Cl:9])=[CH:5][CH:6]=[C:7]([Cl:8])[C:2]=2[N:1]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 103973432-amino-3,6-dichloroPhenolHCID 71342929Ethyl 2-chloroiminoacetate hydrochloride

생성물 1

HCID 103992442-Chloromethyl-4,7-dichlorobenzoxazole수율 86%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-amino-3,6-dichlorophenol (23.91 g, 134 mmol) in methylene chloride (270 mL), solid ethyl chloroiminoacetate hydrogen chloride (31.9 g, 202 mmol) was added. The resultant slurry was stirred at room temperature overnight, then filtered through a plug of Celite, and concentrated under reduced pressure (15 torr). The solid residue was subjected to column chromatography on silica gel (elution with chloroform). Collection and concentration of appropriate fractions yielded 26.6 g (86%) of 2-chloromethyl-4,7-dichlorobenzoxazole.

후처리

  1. filtrationfiltered through a plug of Celite
  2. concentrationconcentrated under reduced pressure (15 torr)
  3. customCollection and concentration of appropriate fractions

출처 및 근거

ORD 기록
ord-68abe93ea1c244cd96fc91713bec7e3d
출처 데이터셋
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05308854

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