2,4,5-T-sodium → HCID 54304081、化合物

HRID 372346ノート

反応式

HRID 372346 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][C:9](=[O:13])[NH:10][CH2:11]Cl.[Cl:14][C:15]1[CH:25]=[C:24]([Cl:26])[C:23]([Cl:27])=[CH:22][C:16]=1[O:17][CH2:18][C:19]([O-:21])=[O:20].[Na+]>C(#N)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][C:9]([NH:10][CH2:11][O:21][C:19](=[O:20])[CH2:18][O:17][C:16]1[CH:22]=[C:23]([Cl:27])[C:24]([Cl:26])=[CH:25][C:15]=1[Cl:14])=[O:13]

参加物

4

反応物 2

HCID 236757872,4,5-T-sodiumHCID 53741911HCID 53741911、化合物

生成物 1

HCID 54304081HCID 54304081、化合物収率 80.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

A solution of 220 g (1 mole) of N-chloromethylcarbamic acid 2-chlorophenyl ester in 1 liter of anhydrous acetonitrile was added dropwise to a suspension of 277.5 g (1 mole) of sodium 2,4,5-trichlorophenoxyacetate in 2 liters of anhydrous acetonitrile. After the exothermic reaction had subsided, the mixture was stirred for a further 15 hours at room temperature. It was then filtered and the filtrate was concentrated in vacuo by distilling off the solvent. The residue was recrystallised from ether/benzine. 354 g (80.6% of theory) of 2-(2,4,5-trichlorophenoxy)-acetic acid 2-chlorophenoxycarbonylaminomethyl ester were obtained in the form of white crystals of melting point 119° C.

後処理

  1. customAfter the exothermic reaction
  2. filtrationIt was then filtered
  3. concentrationthe filtrate was concentrated in vacuo
  4. distillationby distilling off the solvent
  5. customThe residue was recrystallised from ether/benzine

出典と根拠

ORDレコード
ord-a22e5c832c7f4a25b0d984312d95a6cc
出典データセット
uspto-grants-1978_05
特許番号
US04090862

反応ノート

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