Dimethylformamide → 3-{3,5-Dimethyl-4-[6-(5-o-tolyl-[1,3,4]oxadiazol-2-yl)-1H-benzoimidazol-2-yl]-phenyl}-2,2-dimethyl-propionic acid

HRID 1513295노트

반응식

HRID 1513295 반응식
C[O:2][C:3]([C:5]([CH3:28])([CH3:27])[CH2:6][C:7]1[CH:12]=[C:11]([CH3:13])[C:10]([C:14]2[NH:15][C:16]3[CH:22]=[C:21]([C:23]([OH:25])=O)[CH:20]=[CH:19][C:17]=3[N:18]=2)=[C:9]([CH3:26])[CH:8]=1)=[O:4].[NH2:29]C1C=C(C(O)=O)C=CC=1N.COC(=O)C(C)(C)[CH2:44][C:45]1[CH:50]=[C:49](C)[C:48](C=O)=[C:47](C)[CH:46]=1.OOS([O-])=O.[K+].C[N:65]([CH:67]=O)C>O>[CH3:13][C:11]1[CH:12]=[C:7]([CH2:6][C:5]([CH3:27])([CH3:28])[C:3]([OH:2])=[O:4])[CH:8]=[C:9]([CH3:26])[C:10]=1[C:14]1[NH:15][C:16]2[CH:22]=[C:21]([C:23]3[O:25][C:67]([C:46]4[CH:47]=[CH:48][CH:49]=[CH:50][C:45]=4[CH3:44])=[N:65][N:29]=3)[CH:20]=[CH:19][C:17]=2[N:18]=1

참가 물질

7

반응물 5

HCID 6228Dimethylformamide2회HCID 692633,4-Diaminobenzoic acidHCID 23707502Potassium hydroxy sulfiteHCID 669667662-[4-(2-Methoxycarbonyl-2-methyl-propyl)-2,6-dimethyl-phenyl]-3H-benzoimidazole-5-carboxylic acidHCID 86632822Methyl 3-(4-formyl-3,5-dimethylphenyl)-2,2-dimethylpropanoate

생성물 1

HCID 252354593-{3,5-Dimethyl-4-[6-(5-o-tolyl-[1,3,4]oxadiazol-2-yl)-1H-benzoimidazol-2-yl]-phenyl}-2,2-dimethyl-propionic acid

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

2-[4-(2-Methoxycarbonyl-2-methyl-propyl)-2,6-dimethyl -phenyl]-3H-benzoimidazole-5-carboxylic acid. 7.6 g of 3,4-diaminobenzenoic acid was stirred in 120 ml of DMF at room temperature. It was treated with 12.4 g of 3-(4-formyl-3,5-dimethyl-phenyl)-2,2-dimethyl-propionic acid methyl ester (the intermediate A in Example 1-62) followed by an addition of a slurry of 15 g of Oxone in 60 ml of DMF. The reaction was stirred at room temperature for 3 h and 60 mL of water was added and the pH was adjusted to 6. Additional 150 mL of water was added and the resulting precipitates were collected by filtration. The collected precipitates were washed with water and dried under vacuum to afford the title compound.

후처리

  1. customthe resulting precipitates
  2. filtrationwere collected by filtration
  3. customThe collected precipitates
  4. washwere washed with water
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-42dacf1cf08b47f9b477799528c38d48
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217065B2

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