Dicyclohexylcarbodiimide → 5,5-Dimethyl-10-[4-(2-methylpiperidino)butyryloxy]-8-(4-fluorophenyl-1-methylbutyl)-2-(2-propynyl)-1,2,3,4-tetrahydro-5H[1]benzopyrano[3,4-d] pyridine hydrochloride

HRID 2398861

반응식

HRID 2398861 반응식
[CH3:1][C:2]1([CH3:32])[C:24]2[CH2:25][CH2:26][N:27]([CH2:29][C:30]#[CH:31])[CH2:28][C:23]=2[C:5]2[C:6]([OH:22])=[CH:7][C:8]([C:10]([C:15]3[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=3)([CH3:14])[CH2:11][CH2:12][CH3:13])=[CH:9][C:4]=2[O:3]1.[ClH:33].[CH3:34][CH:35]1[CH2:40][CH2:39][CH2:38][CH2:37][N:36]1[CH2:41][CH2:42][CH2:43][C:44](O)=[O:45].C1(N=C=NC2CCCCC2)CCCCC1>C(Cl)Cl.C(OCC)C>[ClH:33].[CH3:32][C:2]1([CH3:1])[C:24]2[CH2:25][CH2:26][N:27]([CH2:29][C:30]#[CH:31])[CH2:28][C:23]=2[C:5]2[C:6]([O:22][C:44](=[O:45])[CH2:43][CH2:42][CH2:41][N:36]3[CH2:37][CH2:38][CH2:39][CH2:40][CH:35]3[CH3:34])=[CH:7][C:8]([C:10]([C:15]3[CH:16]=[CH:17][C:18]([F:21])=[CH:19][CH:20]=3)([CH3:14])[CH2:11][CH2:12][CH3:13])=[CH:9][C:4]=2[O:3]1

참가 물질

6

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 538194395,5dimethyl-10-hydroxy-8-(4-fluorophenyl-1-methylbutyl)-2(2-propynyl)-1,2,3,4-tetrahydro-5H[1]benzopyrano[3,4-d]pyridineHCID 705657274-(2-Methylpiperidin-1-yl)butanoic acid hydrochloride

생성물 1

HCID 888085825,5-Dimethyl-10-[4-(2-methylpiperidino)butyryloxy]-8-(4-fluorophenyl-1-methylbutyl)-2-(2-propynyl)-1,2,3,4-tetrahydro-5H[1]benzopyrano[3,4-d] pyridine hydrochloride

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매2회

실험 절차

A mixture of equimolar quantities of 5,5-dimethyl-10-hydroxy-8-(4-fluorophenyl-1-methylbutyl)-2-(2-propynyl)-1,2,3,4-tetrahydro-5H[1]benzopyrano[3,4-d]pyridine, γ-(2-methylpiperidino)butyric acid hydrochloride and dicyclohexylcarbodiimide in methylene chloride are stirred at room temperature for 16 hours. The reaction mixture is cooled and the solid removed by suction filtration. The methylene chloride is evaporated to give a residue which is dissolved in methylene chloride and diethyl ether. After removing the resulting crude product, the solvents are evaporated and the gummy resin is dried, triturated with diethyl ether, and dried to yield the desired product.

후처리

  1. temperatureThe reaction mixture is cooled
  2. customthe solid removed by suction filtration
  3. customThe methylene chloride is evaporated
  4. customto give a residue which
  5. customAfter removing the resulting crude product
  6. customthe solvents are evaporated
  7. customthe gummy resin is dried
  8. customtriturated with diethyl ether
  9. customdried

출처 및 근거

ORD 기록
ord-2ae359ad2e50465fb1d36a0f77331770
출처 데이터셋
uspto-grants-1977_05
특허 번호
US04025630

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