3-Hydroxyiminomethyl-4-(2,3-dichlorophenyl)pyrrole → Fenpiclonil

HRID 247631

반응식

HRID 247631 반응식
O[N:2]=[CH:3][C:4]1[C:8]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([Cl:15])[C:10]=2[Cl:16])=[CH:7][NH:6][CH:5]=1.ON=CC1NC=C(C2C=CC=C(Cl)C=2Cl)C=1>C(OC(=O)C)(=O)C.C(OCC)(=O)C>[Cl:16][C:10]1[C:11]([Cl:15])=[CH:12][CH:13]=[CH:14][C:9]=1[C:8]1[C:4]([C:3]#[N:2])=[CH:5][NH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 1363937133-Hydroxyiminomethyl-4-(2,3-dichlorophenyl)pyrroleHCID 136393714Hydroxyiminomethyl-4-(2,3-dichlorophenyl)pyrrole

생성물 1

HCID 91724Fenpiclonil

시약·촉매·용매 2

HCID 7918Acetic Anhydride용매HCID 8857Ethyl Acetate용매

실험 절차

3.2 g of the 3-hydroxyiminomethyl-4-(2,3-dichlorophenyl)pyrrole obtained in (b) are kept for 5 hours at c. 100° C. in 50 ml of acetic anhydride, then cooled to room temperature, poured into ice/NaOH, and the resultant mixture is stirred for 2 hours. The precipitate is dissolved in ethyl acetate, washed with water, the exter phase is dried over magnesium sulfate. The residue is purified by column chromatography (silica gel; elution with a 4:1 mixture of toluence/ethyl acetate). Melting point: 149°-151° C.

후처리

  1. washwashed with water
  2. dry with materialthe exter phase is dried over magnesium sulfate
  3. customThe residue is purified by column chromatography (silica gel
  4. washelution
  5. additionwith a 4:1 mixture of toluence/ethyl acetate)

출처 및 근거

ORD 기록
ord-82041719c82b491297a3fe00e6fc208a
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04709053

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