Hydrochloric Acid → 5-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)pentyloxyacetaldehyde O-tert-butyloxime

HRID 1280200

反応式

HRID 1280200 の反応式
[Cl:1][C:2]1[CH:17]=[C:16]([O:18][CH2:19][CH:20]=[C:21]([Cl:23])[Cl:22])[CH:15]=[C:14]([Cl:24])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][O:10][CH2:11][CH:12]=O.Cl.[C:26]([O:30][NH2:31])([CH3:29])([CH3:28])[CH3:27].Cl>N1C=CC=CC=1>[C:26]([O:30][N:31]=[CH:12][CH2:11][O:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][O:4][C:3]1[C:14]([Cl:24])=[CH:15][C:16]([O:18][CH2:19][CH:20]=[C:21]([Cl:22])[Cl:23])=[CH:17][C:2]=1[Cl:1])([CH3:29])([CH3:28])[CH3:27]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 2777906O-tert-butylhydroxylamine hydrochlorideHCID 540452085-(2,6-Dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)pentyloxyacetaldehyde

生成物 1

HCID 544557595-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)pentyloxyacetaldehyde O-tert-butyloxime収率 92%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a mixture of 0.42 g of 5-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)pentyloxyacetaldehyde and 10 ml of pyridine was added 0.13 g of O-tert-butylhydroxylamine hydrochloride. After stirring at room temperature for 24 hours, the reaction mixture was poured into diluted hydrochloric acid, and extracted twice with diethyl ether. The diethyl ether layers were combined, washed with water, dried over anhydrous magnesium sulfate, and concentrated to give a crude product. This crude product was subjected to silica gel chromatography, which afforded 0.45 g (yield, 92%) of 5-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)pentyloxyacetaldehyde O-tert-butyloxime, nD25.2 1.5185.

後処理

  1. extractionextracted twice with diethyl ether
  2. washwashed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customto give a crude product

出典と根拠

ORDレコード
ord-164a9441b0c04990bade27c6e346833e
出典データセット
uspto-grants-2002_09
特許番号
US06448444B1

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