(2,4-Dichlorophenoxy)acetyl chloride → 3-[(1-Ethylpropyl)amino]-6-methyl-2,4-dinitrobenzyl (2,4-dichlorophenoxy)acetate

HRID 1388079

反応式

HRID 1388079 の反応式
[CH2:1]([CH:3]([NH:6][C:7]1[C:8]([N+:19]([O-:21])=[O:20])=[C:9]([C:12]([CH3:18])=[CH:13][C:14]=1[N+:15]([O-:17])=[O:16])[CH2:10][OH:11])[CH2:4][CH3:5])[CH3:2].[Cl:22][C:23]1[CH:33]=[C:32]([Cl:34])[CH:31]=[CH:30][C:24]=1[O:25][CH2:26][C:27](Cl)=[O:28]>C1C=CC=CC=1.CCOCC>[Cl:22][C:23]1[CH:33]=[C:32]([Cl:34])[CH:31]=[CH:30][C:24]=1[O:25][CH2:26][C:27]([O:11][CH2:10][C:9]1[C:12]([CH3:18])=[CH:13][C:14]([N+:15]([O-:17])=[O:16])=[C:7]([NH:6][CH:3]([CH2:4][CH3:5])[CH2:1][CH3:2])[C:8]=1[N+:19]([O-:21])=[O:20])=[O:28]

参加物

5

反応物 2

HCID 69887(2,4-Dichlorophenoxy)acetyl chlorideHCID 1566883-((1-Ethylpropyl)amino)-6-methyl-2,4-dinitrobenzyl alcohol

生成物 1

HCID 129407643-[(1-Ethylpropyl)amino]-6-methyl-2,4-dinitrobenzyl (2,4-dichlorophenoxy)acetate

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 3283Diethyl Ether溶媒

反応条件

温度
60 °C

実験手順

3-[(1-Ethylpropyl)amino]-6-methyl-2,4-dinitrobenzyl alcohol (2.0 g; 0.007 mol) and 2,4-dichlorophenoxyacetyl chloride (used in excess over theory) are dissolved in benzene, and the solution stirred at 60° C. until tlc (silica gel-benzene) indicates the reaction to be complete. The reaction mixture is then cooled down, diluted with ether, and washed with dilute sodium bicarbonate solution until the washings became alkaline. The organic layer is then separated, dried over magnesium sulfate, and evaporated to afford a liquid residue, which solidifies gradually (3.3 g; 94%). Recrystallization of this solid from methanol affords 1.4 g of title product, melting point 103°-106° C.

後処理

  1. customthe reaction
  2. temperatureThe reaction mixture is then cooled down
  3. washwashed with dilute sodium bicarbonate solution until the washings
  4. customThe organic layer is then separated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customto afford a liquid residue, which
  8. customRecrystallization of this solid from methanol

出典と根拠

ORDレコード
ord-35a06acdc4b8426fbb81651fdf2f46c2
出典データセット
uspto-grants-1984_02
特許番号
US04430114

関連ノート

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