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

HRID 977847ノート

反応式

HRID 977847 の反応式
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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 19966206HCID 19966206、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c8dc89b5f2de48b1be2a32b87a266166
出典データセット
uspto-grants-1997_03
特許番号
US05614550

反応ノート

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