1,3,5-Tributyl-4-methylamino-1,2,4-triazolium chloride → 1,3,5-Tributyl-4-methylamino-1,2,4-triazolium (1,1-dimethoxyethyl)methylphosphinate

HRID 1759175노트

반응식

HRID 1759175 반응식
[CH3:1][O:2][C:3]([P:7]([CH3:10])(=[O:9])[O-:8])([O:5][CH3:6])[CH3:4].[Na+].[Cl-].[CH2:13]([N+:17]1[N:18]=[C:19]([CH2:28][CH2:29][CH2:30][CH3:31])[N:20]([NH:26][CH3:27])[C:21]=1[CH2:22][CH2:23][CH2:24][CH3:25])[CH2:14][CH2:15][CH3:16]>>[CH3:1][O:2][C:3]([P:7]([CH3:10])(=[O:8])[O-:9])([O:5][CH3:6])[CH3:4].[CH2:13]([N+:17]1[N:18]=[C:19]([CH2:28][CH2:29][CH2:30][CH3:31])[N:20]([NH:26][CH3:27])[C:21]=1[CH2:22][CH2:23][CH2:24][CH3:25])[CH2:14][CH2:15][CH3:16]

참가 물질

3

반응물 2

HCID 705234511,3,5-Tributyl-4-methylamino-1,2,4-triazolium chlorideHCID 86738481HCID 86738481, 화합물

생성물 1

HCID 867384911,3,5-Tributyl-4-methylamino-1,2,4-triazolium (1,1-dimethoxyethyl)methylphosphinate수율 73.4%

실험 절차

By the procedure of Example 50 the product of Example 18 (3.8 g) and 1,3,5-tributyl-4-methylamino-1,2,4-triazolium chloride (5.7 g) were mixed and the resulting sodium chloride filtered off. The filtrate was evaporated in vacuo and the residual oil treated with acetone. Unreacted phosphinate (0.3 g) was filtered off and the filtrate evaporated in vacuo, finally at the oil pump, to give the required salt as an amber oil (6.0 g). The nmr spectrum was in agreement with the structure.

후처리

  1. filtrationthe resulting sodium chloride filtered off
  2. customThe filtrate was evaporated in vacuo
  3. additionthe residual oil treated with acetone
  4. filtrationUnreacted phosphinate (0.3 g) was filtered off
  5. customthe filtrate evaporated in vacuo, finally at the oil pump

출처 및 근거

ORD 기록
ord-248e39af3a1e480d938935efaea6cf96
출처 데이터셋
uspto-grants-1982_07
특허 번호
US04339443

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