Hydroxyamine hydrochloride → (NZ)-N-[(4-chloro-2-fluoro-5-methoxyphenyl)-[4-(4-chlorophenoxy)-2-propylphenyl]methylidene]hydroxylamine

HRID 1172827노트

반응식

HRID 1172827 반응식
[Cl:1][C:2]1[CH:29]=[CH:28][C:5]([O:6][C:7]2[CH:12]=[CH:11][C:10]([C:13]([C:15]3[CH:20]=[C:19]([O:21][CH3:22])[C:18]([Cl:23])=[CH:17][C:16]=3[F:24])=O)=[C:9]([CH2:25][CH2:26][CH3:27])[CH:8]=2)=[CH:4][CH:3]=1.Cl.[NH2:31][OH:32].C([O-])(=O)C.[Na+]>C(O)C>[Cl:1][C:2]1[CH:29]=[CH:28][C:5]([O:6][C:7]2[CH:12]=[CH:11][C:10](/[C:13](/[C:15]3[CH:20]=[C:19]([O:21][CH3:22])[C:18]([Cl:23])=[CH:17][C:16]=3[F:24])=[N:31]/[OH:32])=[C:9]([CH2:25][CH2:26][CH3:27])[CH:8]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 68689947[4-(4-Chlorophenoxy)-2-propylphenyl][4-chloro-2-fluoro-5-methoxyphenyl]methanone

생성물 1

HCID 87541464(NZ)-N-[(4-chloro-2-fluoro-5-methoxyphenyl)-[4-(4-chlorophenoxy)-2-propylphenyl]methylidene]hydroxylamine

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

A mixture of the product from Step 3 (1.4 g, 3.2 mmol), hydroxylamine hydrochloride (2.2 g, 32 mmol) and sodium acetate (2.6 g, 32 mmol) in ethanol (30 mL) was stirred in a sealed tube at 60° C. for 72 h. The precipitate was filtered off and the filtrate was concentrated. The residue was purified by chromatography on silica gel to give the oxime product.

후처리

  1. filtrationThe precipitate was filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-03cfe079c7e142128b5e3fbbf56af84c
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834036B2

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