Hydrochloric Acid → HCID 10239323、化合物

HRID 1373855ノート

反応式

HRID 1373855 の反応式
O1CCCC1.[OH-].[Na+].[CH:8]1([C:14]2[CH:45]=[CH:44][C:17]([CH2:18][O:19][C:20]3[CH:25]=[CH:24][C:23]([C:26]4[N:27]=[C:28]([N:31]([CH2:33][C:34]5[CH:43]=[CH:42][C:37]([C:38]([O:40]C)=[O:39])=[CH:36][CH:35]=5)[CH3:32])[S:29][CH:30]=4)=[CH:22][CH:21]=3)=[CH:16][CH:15]=2)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.Cl>O.CO>[CH:8]1([C:14]2[CH:45]=[CH:44][C:17]([CH2:18][O:19][C:20]3[CH:25]=[CH:24][C:23]([C:26]4[N:27]=[C:28]([N:31]([CH2:33][C:34]5[CH:35]=[CH:36][C:37]([C:38]([OH:40])=[O:39])=[CH:42][CH:43]=5)[CH3:32])[S:29][CH:30]=4)=[CH:22][CH:21]=3)=[CH:16][CH:15]=2)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 23023934HCID 23023934、化合物

生成物 1

HCID 10239323HCID 10239323、化合物収率 99.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Tetrahydrofuran (250 ml), methanol (250 ml) and a 2N-aqueous sodium hydroxide solution (95.0 ml, 190 mmol) were added to methyl 4-(N-(4-(4-(4-cyclohexylbenzyloxy)phenyl)-2-thiazolyl)-N-methylaminomethyl)benzoate (50.0 g, 94.9 mmol) obtained in Example 2(4), and the mixture was heated under reflux for 40 min under an argon atmosphere. Water (310 ml) was added to the reaction mixture and the mixture was cooled to room temperature. 2N-Hydrochloric acid (95.0 ml, 190 mmol) was added dropwise and the mixture was stirred for 90 min. The resulting crystals were collected by filtration, washed with water (700 mL) and dried to give the title compound (48.5 g, yield 99.7%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 40 min under an argon atmosphere
  3. filtrationThe resulting crystals were collected by filtration
  4. washwashed with water (700 mL)
  5. customdried

出典と根拠

ORDレコード
ord-4bc92efff09944549318d0c44a96248f
出典データセット
uspto-grants-2007_01
特許番号
US07163952B2

反応ノート

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