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Cyclohexanol → Cyclohexyl 5-(2,4-dichlorophenoxy)-2-nitrobenzoate

HRID 1414148
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HRID 1414148 반응식
[CH:1]1([OH:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[Cl:15][C:16]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:17]=1[O:18][C:19]1[CH:20]=[CH:21][C:22]([N+:28]([O-:30])=[O:29])=[C:23]([CH:27]=1)[C:24](Cl)=[O:25].Cl.C(N(CC)CC)C>C1(C)C=CC=CC=1.C(OCC)C>[Cl:15][C:16]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:17]=1[O:18][C:19]1[CH:20]=[CH:21][C:22]([N+:28]([O-:30])=[O:29])=[C:23]([CH:27]=1)[C:24]([O:7][CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 7966CyclohexanolHCID 8471TriethylamineHCID 11130Triethylamine hydrochlorideHCID 130202985-(2,4-Dichlorophenoxy)-2-nitrobenzoyl chloride

생성물 1

HCID 21486094Cyclohexyl 5-(2,4-dichlorophenoxy)-2-nitrobenzoate

시약·촉매·용매 2

HCID 1140Toluene
용매
HCID 3283Diethyl Ether용매

실험 절차

To a stirred solution of cyclohexanol (1.05g., 0.0105 mole) and triethylamine (1.10g., 0.011 mole) in toluene (30 ml.) was added 5-(2',4'-dichlorophenoxy)-2-nitrobenzoyl chloride (3.47g., 0.01 mole). A precipitate of triethylamine hydrochloride occurred immediately. The reaction solution was heated to reflux for one hour, cooled and diluted with diethyl ether (150 ml.). After filtering the triethylamine hydrochloride, the solvent was evaporated to give 4.1g. of a brown oil. A small amount of additional precipitate was filtered off. The ether was again stripped to yield 3.5g. of brown oil.

후처리

  1. temperatureThe reaction solution was heated
  2. temperatureto reflux for one hour
  3. temperaturecooled
  4. filtrationAfter filtering the triethylamine hydrochloride
  5. customthe solvent was evaporated
  6. customto give 4.1g
  7. filtrationA small amount of additional precipitate was filtered off
  8. customto yield 3.5g

출처 및 근거

ORD 기록
ord-c9e2f7d53ff048e39212d9718131f103
출처 데이터셋
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04001005

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