Hydrochloric Acid → N-(2-t-Butyl-5-{3-[2-(1-imidazolyl)acetoxy]-4-cyclohexylbutyl}phenyl)-2-(9H-xanthen-9-yl)acetamide hydrochloride

HRID 977847노트

반응식

HRID 977847 반응식
O1CCOCC1.[ClH:7].[C:8]([C:12]1[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][CH:20]([O:28][C:29](=[O:36])[CH2:30][N:31]2[CH:35]=[CH:34][N:33]=[CH:32]2)[CH2:21][CH:22]2[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]2)=[CH:14][C:13]=1[NH:37][C:38](=[O:54])[CH2:39][CH:40]1[C:53]2[CH:52]=[CH:51][CH:50]=[CH:49][C:48]=2[O:47][C:46]2[C:41]1=[CH:42][CH:43]=[CH:44][CH:45]=2)([CH3:11])([CH3:10])[CH3:9]>C(OCC)C>[ClH:7].[C:8]([C:12]1[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][CH:20]([O:28][C:29](=[O:36])[CH2:30][N:31]2[CH:35]=[CH:34][N:33]=[CH:32]2)[CH2:21][CH:22]2[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]2)=[CH:14][C:13]=1[NH:37][C:38](=[O:54])[CH2:39][CH:40]1[C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][C:46]=2[O:47][C:48]2[C:53]1=[CH:52][CH:51]=[CH:50][CH:49]=2)([CH3:11])([CH3:9])[CH3:10]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 19966206HCID 19966206, 화합물

생성물 1

HCID 19966205N-(2-t-Butyl-5-{3-[2-(1-imidazolyl)acetoxy]-4-cyclohexylbutyl}phenyl)-2-(9H-xanthen-9-yl)acetamide hydrochloride수율 85%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

200 μl of a 4N dioxane solution of hydrogen chloride were added to a solution of 339 mg (0.54 mmol) of N-(2-t-butyl-5-{3-[2-(1-imidazolyl)acetoxy]-4-cyclohexylbutyl}phenyl)-2-(9H-xanthen-9-yl)acetamide [prepared as described in step (i) above] in 3 ml of diethyl ether, and the crystals which precipitated were collected by filtration and washed with diethyl ether. The crystals were purified by high performance liquid chromatography through ODS (120 A, φ30 mm×250 mm) using a 3:1 by volume mixture of acetonitrile and water as the eluent, to give a gel. This gel was crystallized by trituration with diethyl ether, to give 170 mg (yield 85%) of the title compound as colorless crystals, melting at 125°-133° C.

후처리

  1. customthe crystals which precipitated
  2. filtrationwere collected by filtration
  3. washwashed with diethyl ether
  4. customThe crystals were purified by high performance liquid chromatography through ODS (120 A, φ30 mm×250 mm)
  5. additionby volume mixture of acetonitrile and water as the eluent
  6. customto give a gel
  7. customThis gel was crystallized by trituration with diethyl ether

출처 및 근거

ORD 기록
ord-c8dc89b5f2de48b1be2a32b87a266166
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05614550

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