Dicyclohexano-18-crown-6 → HCID 57261350, 화합물

HRID 341968

반응식

HRID 341968 반응식
[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:13]([O:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH3:22])[CH:16]=2)=[C:12]([NH:23][S:24]([C:27]2[CH:32]=[CH:31][C:30]([C:33]([CH3:36])([CH3:35])[CH3:34])=[CH:29][CH:28]=2)(=[O:26])=[O:25])[N:11]=[C:10]([CH:37]=[O:38])[N:9]=1)(=[O:3])[CH3:2].C1CC2[O:45]CCOCCOC3C(OCCOCCOC2CC1)CCCC3.[Mn]([O-])(=O)(=O)=O.[K+]>C1C=CC=CC=1>[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:13]([O:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH3:22])[CH:16]=2)=[C:12]([NH:23][S:24]([C:27]2[CH:28]=[CH:29][C:30]([C:33]([CH3:34])([CH3:36])[CH3:35])=[CH:31][CH:32]=2)(=[O:25])=[O:26])[N:11]=[C:10]([C:37]([OH:45])=[O:38])[N:9]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 85955Dicyclohexano-18-crown-6HCID 516875Potassium PermanganateHCID 57295961HCID 57295961, 화합물

생성물 1

HCID 57261350HCID 57261350, 화합물수율 32.4%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

0.27 g of 2-[6-(4-tert.butyl-phenylsulphonylamino)-2-formyl-5-(3-methoxy-phenoxy)-pyrimidin-4-yloxy]-ethyl acetate and 0.19 g of dicyclohexyl-18-crown-6 in 15 ml of benzene were stirred with 0.078 g of potassium permanganate at 2000 for 16 hours. The reaction mixture was partitioned between toluene and water. The organic phase was dried and evaporated, and the residue was purified over silica gel with chloroform-methanol. 0.09 g of 4-(2-acetoxy-ethoxy)-6-(4-tert.butyl-phenylsulphonylamino)-5-(3-methoxy-phenoxy)-pyrimidine-2-carboxylic acid was obtained as a foam, MS: (M-H)- 558.

후처리

  1. customThe reaction mixture was partitioned between toluene and water
  2. customThe organic phase was dried
  3. customevaporated
  4. customthe residue was purified over silica gel with chloroform-methanol

출처 및 근거

ORD 기록
ord-75af54caab9b4a82a6a91bc5afaf2108
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05856484

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