2,4,5-T-sodium → HCID 54304081, 화합물

HRID 372346노트

반응식

HRID 372346 반응식
[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]

참가 물질

4

반응물 2

HCID 236757872,4,5-T-sodiumHCID 53741911HCID 53741911, 화합물

생성물 1

HCID 54304081HCID 54304081, 화합물수율 80.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a22e5c832c7f4a25b0d984312d95a6cc
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04090862

반응 노트

불러오는 중…