Dicyclohexano-18-crown-6 → HCID 57261350、化合物

HRID 341968

反応式

HRID 341968 の反応式
[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]

参加物

5

反応物 3

HCID 85955Dicyclohexano-18-crown-6HCID 516875Potassium PermanganateHCID 57295961HCID 57295961、化合物

生成物 1

HCID 57261350HCID 57261350、化合物収率 32.4%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-75af54caab9b4a82a6a91bc5afaf2108
出典データセット
uspto-grants-1999_01
特許番号
US05856484

関連ノート

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