Sodium Hydroxide → HCID 18668744, 화합물

HRID 1058624노트

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HRID 1058624 반응식
O([C:8]1[C:17]2[N:18]=[CH:19][N:20]([CH2:21][CH2:22][CH:23]3[CH2:28][CH2:27][N:26]([C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])[CH2:25][CH2:24]3)[C:16]=2[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N:9]=1)C1C=CC=CC=1.C([O-])(=O)C.[NH4+:40].[OH-].[Na+]>O>[NH2:40][C:8]1[C:17]2[N:18]=[CH:19][N:20]([CH2:21][CH2:22][CH:23]3[CH2:28][CH2:27][N:26]([C:29]([O:31][C:32]([CH3:33])([CH3:35])[CH3:34])=[O:30])[CH2:25][CH2:24]3)[C:16]=2[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N:9]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 517165Ammonium AcetateHCID 18668801tert-Butyl 4-[2-(4-phenoxy-1H-imidazo[4,5-c]quinolin-1-yl)ethyl]-1-piperidinecarboxylate

생성물 1

HCID 18668744HCID 18668744, 화합물수율 51.1%

시약·촉매·용매 1

HCID 962Water용매

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온도
140 °C

실험 절차

A mixture of 4.40 g of tert-butyl 4-[2-(4-phenoxy-1H-imidazo[4,5-c]-quinolin-1-yl)ethyl]-1-piperidinecarboxylate and 34.5 g of ammonium acetate was stirred at 140° C. for 3 hours. The reaction mixture was added with water, adjusted to pH 9 with 10% aqueous sodium hydroxide solution, and extracted with methylene chloride. The extract was washed with saturated brine, and dried, and then the solvent was evaporated. The resulting residue was purified by alumina column chromatography using methylene chloride—methanol (100:1 to 20:1) as eluting solvents, and washed with diisopropyl ether to give 1.88 g of colorless crystals. Recrystallization from ethyl acetate gave colorless crystals having the melting point of from 193 to 193.5° C.

후처리

  1. extractionextracted with methylene chloride
  2. washThe extract was washed with saturated brine
  3. customdried
  4. customthe solvent was evaporated
  5. customThe resulting residue was purified by alumina column chromatography
  6. washas eluting solvents
  7. washwashed with diisopropyl ether

출처 및 근거

ORD 기록
ord-1000bc96acc84b4ba3b3e3ed836bdeec
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06518265B1

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