Hydrochloric Acid → HCID 10239323, 화합물

HRID 1373855노트

반응식

HRID 1373855 반응식
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

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 23023934HCID 23023934, 화합물

생성물 1

HCID 10239323HCID 10239323, 화합물수율 99.7%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-4bc92efff09944549318d0c44a96248f
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07163952B2

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