Triethylamine → 3-Tetrahydrofuryl 2-nitro-5-(2-cyano-4-trifluoromethylphenoxy)benzoate

HRID 2290686노트

반응식

HRID 2290686 반응식
[OH:1][CH:2]1[CH2:6][CH2:5][O:4][CH2:3]1.C(N(CC)CC)C.[N+:14]([C:17]1[CH:25]=[CH:24][C:23]([O:26][C:27]2[CH:32]=[CH:31][C:30]([C:33]([F:36])([F:35])[F:34])=[CH:29][C:28]=2[C:37]#[N:38])=[CH:22][C:18]=1[C:19](Cl)=[O:20])([O-:16])=[O:15]>C1(C)C=CC=CC=1>[N+:14]([C:17]1[CH:25]=[CH:24][C:23]([O:26][C:27]2[CH:32]=[CH:31][C:30]([C:33]([F:34])([F:35])[F:36])=[CH:29][C:28]=2[C:37]#[N:38])=[CH:22][C:18]=1[C:19]([O:1][CH:2]1[CH2:6][CH2:5][O:4][CH2:3]1)=[O:20])([O-:16])=[O:15]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 99603-Furanol, tetrahydro-HCID 202299225-[2-Cyano-4-(trifluoromethyl)phenoxy]-2-nitrobenzoyl chloride

생성물 1

HCID 137313093-Tetrahydrofuryl 2-nitro-5-(2-cyano-4-trifluoromethylphenoxy)benzoate

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

3-Hydroxytetrahydrofuran (0.04 mole), toluene (50 ml) and triethylamine (0.04 mole) are charged into a glass reaction vessel equipped with a mechanical stirrer and addition funnel. A solution of 2-nitro-5-(2-cyano-4-trifluoromethylphenoxy)benzoyl chloride (0.04 mole) in toluene (20 ml) is slowly added at room temperature with stirring. After the addition is completed, stirring is continued for a period of about eight hours. After this time, the reaction mixture is washed with water and dried over anhydrous magnesium sulfate. The dried solution is then stripped of solvent under reduced pressure leaving a residue. This residue is purified by silica gel chromatography using toluene and ethyl acetate/toluene mixture as the eluant to yield the desired product 3-tetrahydrofuryl 2-nitro-5-(2-cyano-4-trifluoromethylphenoxy)benzoate.

후처리

  1. customequipped with a mechanical stirrer and addition funnel
  2. additionAfter the addition
  3. stirringstirring
  4. washAfter this time, the reaction mixture is washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customleaving a residue
  7. customThis residue is purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-9d31047fc5b3409ea041bcc194bae545
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04618359

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