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2-Phenylglutaric anhydride → HCID 88678971, 화합물

HRID 280350
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HRID 280350 반응식
[NH2:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][CH:7]([NH:10][C:11]2[N:15]([CH2:16][C:17]3[O:18][CH:19]=[CH:20][CH:21]=3)[C:14]3[CH:22]=[CH:23][CH:24]=[CH:25][C:13]=3[N:12]=2)[CH2:6][CH2:5]1.C1(C2CCC(=O)[O:34][C:33]2=O)C=CC=CC=1>CN(C)C=O>[OH2:18].[O:18]1[CH:19]=[CH:20][CH:21]=[C:17]1[CH2:16][N:15]1[C:14]2[CH:22]=[CH:23][CH:24]=[CH:25][C:13]=2[N:12]=[C:11]1[NH:10][CH:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH2:2][NH:1][CH:33]=[O:34])[CH2:5][CH2:6]1.[O:18]1[CH:19]=[CH:20][CH:21]=[C:17]1[CH2:16][N:15]1[C:14]2[CH:22]=[CH:23][CH:24]=[CH:25][C:13]=2[N:12]=[C:11]1[NH:10][CH:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH2:2][NH:1][CH:33]=[O:34])[CH2:5][CH2:6]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 962932-Phenylglutaric anhydrideHCID 13588039N-[1-(2-aminoethyl)-4-piperidinyl]-1-(2-furanylmethyl)-1H-benzimidazol-2-amine

생성물 1

HCID 88678971HCID 88678971, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

반응 조건

온도
50 °C

실험 절차

A mixture of 5.09 parts of N-[1-(2-aminoethyl)-4-piperidinyl]-1-(2-furanylmethyl)-1H-benzimidazol-2-amine and 54 parts of N,N-dimethylformamide was stirred and heated at 50° C. and there was added dropwise a solution of 2.8 parts of dihydro-3-phenyl-2H-pyran-2,6(3H)dione in 18 parts of N,N-dimethylformamide. Upon completion, stirring was continued overnight at 50° C. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was from a mixture of acetonitrile and 2,2'-oxybispropane, yielding 1.8 parts of N-[2-[4-[[1-(2-furanylmethyl)-1H-benzimidazol-2-yl]amino]-1-piperidinyl]ethyl]formamide hemihydrate; mp. 125.2° C. (compound 46).

후처리

  1. stirringUpon completion, stirring
  2. customThe residue was purified by column chromatography over silica gel using
  3. additiona mixture of trichloromethane and methanol
  4. customThe pure fractions were collected
  5. customthe eluent was evaporated
  6. additionThe residue was from a mixture of acetonitrile and 2,2'-oxybispropane

출처 및 근거

ORD 기록
ord-860d3a453ea64aa4a5de0f27c839b1e0
출처 데이터셋
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04588722

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