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Water → HCID 20061086, 화합물

HRID 2399033
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HRID 2399033 반응식
O.Cl.[N+:3]([C:6]1[CH:7]=[C:8]([CH:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=2)[OH:14])[CH:9]=[CH:10][C:11]=1[Cl:12])([O-:5])=[O:4]>[O-2].[O-2].[O-2].[Cr+6].C(O)(=O)C>[N+:3]([C:6]1[CH:7]=[C:8]([CH:9]=[CH:10][C:11]=1[Cl:12])[C:13]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=1)=[O:14])([O-:5])=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 962WaterHCID 68117057HCID 68117057, 화합물

생성물 1

HCID 20061086HCID 20061086, 화합물

시약·촉매·용매 2

HCID 10219390chromium (VI) trioxide촉매HCID 176Acetic Acid용매

실험 절차

A solution of 27 g. (0.27 mol) of chromium trioxide in 250 ml. of water was added to a solution of 80 g. (0.266 mol) of 3-nitro-4-chlorophenyl-2-pyridyl methanol hydrochloride in 800 ml. of 75% acetic acid at 45° C. and the mixture was heated to 75° C. for 1 hr. The resulting dark green solution was poured into 3 liters of ice-water. The resulting product was filtered off, washed with water, dissolved in methylene chloride, dried with sodium sulfate and concentrated in vacuo to yield 2-(3-nitro-4-chlorobenzoyl)pyridine as white microneedles, mp. 98° -99° C. (cyclohexane).

후처리

  1. filtrationThe resulting product was filtered off
  2. washwashed with water
  3. dissolutiondissolved in methylene chloride
  4. dry with materialdried with sodium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b704094cdabd4a09b01f0033dd302ef1
출처 데이터셋
uspto-grants-1977_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04026936

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