Sodium Phosphate, Dibasic → HCID 18415667, 화합물

HRID 990620노트

반응식

HRID 990620 반응식
Br[C:2]([F:19])([F:18])[S:3]([C:6]1[N:10]=[CH:9][N:8]([C:11](=[O:17])[N:12]([CH2:15][CH3:16])[CH2:13][CH3:14])[N:7]=1)(=[O:5])=[O:4].[CH2:20](SC1SCCN=1)[CH:21]=[CH2:22].P([O-])([O-])(O)=O.[Na+].[Na+].S(S([O-])=O)([O-])=O.[Na+].[Na+]>CN(C)C=O.O>[CH2:13]([N:12]([CH2:15][CH3:16])[C:11]([N:8]1[CH:9]=[N:10][C:6]([S:3]([C:2]([F:19])([F:18])[CH2:22][CH:21]=[CH2:20])(=[O:5])=[O:4])=[N:7]1)=[O:17])[CH3:14]

참가 물질

7

반응물 4

HCID 24203Sodium Phosphate, DibasicHCID 24489Sodium DithioniteHCID 771192-(Allylthio)-2-thiazolineHCID 12056494HCID 12056494, 화합물

생성물 1

HCID 18415667HCID 18415667, 화합물수율 29%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of 10 g (0.028 mol) 3-(bromodifluoromethylsulfonyl)-1-(N,N-diethylcarbamoyl)-1,2,4-triazole, prepared as in Example 1, and 8.81 g (0.055 mol) 2-(2-propenylthio)-2-thiazoline in a mixture of 30 ml dimethylformamide and 20 ml water at 0° C., was added 5.9 g (0.042 mol) sodium hydrogen phosphate and 7.23 g (0.042 mol) sodium dithionite. After 2 h, the reaction mixture was diluted with 100 ml water and extracted with ethyl acetate (3×100 ml). The combined resulting organic layers were washed with saturated sodium chloride solution, dried over MgSO4 and evaporated. Preparative LC purification of the residue with 40% ethyl acetate-hexane gave 2.59 g (29% yield) of the desired product as a colorless oil having n D 25 = 1.4896 .

후처리

  1. extractionextracted with ethyl acetate (3×100 ml)
  2. customThe combined resulting organic layers
  3. washwere washed with saturated sodium chloride solution
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. customPreparative LC purification of the residue with 40% ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-29119bf906ff40a8b7a9d9e6944e43cb
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06461997B1

반응 노트

불러오는 중…