Triethylamine → 3,6-dichloro-N-[4-(dimethylphosphoryl)phenyl]-1,2,4-triazin-5-amine

HRID 1472107노트

반응식

HRID 1472107 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([P:8](=[O:11])([CH3:10])[CH3:9])=[CH:4][CH:3]=1.[Cl:12][C:13]1[N:14]=[N:15][C:16]([Cl:20])=[C:17](Cl)[N:18]=1.C(N(CC)CC)C>C(Cl)Cl>[Cl:12][C:13]1[N:14]=[N:15][C:16]([Cl:20])=[C:17]([NH:1][C:2]2[CH:3]=[CH:4][C:5]([P:8]([CH3:9])([CH3:10])=[O:11])=[CH:6][CH:7]=2)[N:18]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 122624033,5,6-Trichloro-1,2,4-triazineHCID 206345534-(Dimethylphosphoryl)aniline

생성물 1

HCID 866688243,6-dichloro-N-[4-(dimethylphosphoryl)phenyl]-1,2,4-triazin-5-amine

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 4-amino-dimethylphenylphosphine oxide (1.6 mmol) and 3,5,6-trichloro-1,2,4-triazine (1.6 mmol) in CH2Cl2, is added triethylamine (2 mmol). The reaction mixture is allowed to cool to room temperature, dissolved in dichloromethane and washed with an aqueous solution of Na2CO3. The dichloromethane extract is dried over MgSO4 and evaporated. The crude product is purified by Prep-HPLC.

후처리

  1. washwashed with an aqueous solution of Na2CO3
  2. extractionThe dichloromethane extract
  3. dry with materialis dried over MgSO4
  4. customevaporated
  5. customThe crude product is purified by Prep-HPLC

출처 및 근거

ORD 기록
ord-b5173b9c7aa644cda798faf1be963748
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09012462B2

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