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Methanol → HCID 19095952, 화합물

HRID 486764
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HRID 486764 반응식
C[Si](C)(C)[NH:3][Si](C)(C)C.CO.[C:12]([O:16][C:17]([N:19]1[CH2:23][CH2:22][C:21]2([CH2:52][CH2:51][N:26]3[C:27]4[C:32]([C:33]([C:34]5[C:35](=[O:50])O[C:37](=[O:49])[C:38]=5[C:39]5[C:47]6[C:42](=[CH:43][CH:44]=[CH:45][CH:46]=6)[N:41]([CH3:48])[CH:40]=5)=[C:25]3[CH2:24]2)=[CH:31][CH:30]=[CH:29][CH:28]=4)[CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].O>CN(C=O)C>[C:12]([O:16][C:17]([N:19]1[CH2:23][CH2:22][C:21]2([CH2:52][CH2:51][N:26]3[C:27]4[C:32]([C:33]([C:34]5[C:35](=[O:50])[NH:3][C:37](=[O:49])[C:38]=5[C:39]5[C:47]6[C:42](=[CH:43][CH:44]=[CH:45][CH:46]=6)[N:41]([CH3:48])[CH:40]=5)=[C:25]3[CH2:24]2)=[CH:31][CH:30]=[CH:29][CH:28]=4)[CH2:20]1)=[O:18])([CH3:13])([CH3:14])[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 13838HexamethyldisilazaneHCID 19095966HCID 19095966, 화합물

생성물 1

HCID 19095952HCID 19095952, 화합물수율 58.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4.09 g of 1,1,1,3,3,3-hexamethyldisilazane and 0.41 g of methanol was added to a solution of 1.40 g of 3-[1'-(tert.butoxycarbonyl)-7,9-dihydrospiro[pyrido[1,2-a]indole-8(6H),3'-pyrrolidin]-10-yl]-4-(1-methyl-3-indolyl)furan-2,5-dione in 25 ml of dry DMF and stirred for 16 hours. The mixture was poured into 100 ml of water and extracted with ethyl acetate. The ethyl acetate extracts were washed with sodium chloride solution, dried and concentrated. There were obtained 820 mg of 3-[1'-(tert.butoxycarbonyl)-7,9-dihydrospiro[pyrido-[1,2-a]indole-8(6H).3'-pyrrolidin]-10-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione after chromatography on silica gel using dichloromethane/methanol (9:1) for the elution.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate extracts were washed with sodium chloride solution
  3. customdried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f45da85435024cd6b61b1170aa4375f6
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05292747

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