Potassium Carbonate → HCID 10139190, 화합물

HRID 1835582노트

반응식

HRID 1835582 반응식
C([O:4][C:5]1[CH:6]=[C:7]([O:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]3[N:22]([CH:23]4[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]4)[C:21]4[CH:29]=[CH:30][C:31]([C:33]([O:35][CH2:36][CH3:37])=[O:34])=[CH:32][C:20]=4[N:19]=3)=[CH:14][CH:13]=2)[CH:8]=[CH:9][CH:10]=1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO.O1CCCC1>[CH:23]1([N:22]2[C:21]3[CH:29]=[CH:30][C:31]([C:33]([O:35][CH2:36][CH3:37])=[O:34])=[CH:32][C:20]=3[N:19]=[C:18]2[C:15]2[CH:14]=[CH:13][C:12]([O:11][C:7]3[CH:8]=[CH:9][CH:10]=[C:5]([OH:4])[CH:6]=3)=[CH:17][CH:16]=2)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]1

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 10228675HCID 10228675, 화합물

생성물 1

HCID 10139190HCID 10139190, 화합물수율 97.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl 2-[4-(3-acetoxyphenyloxy)phenyl]-1-cyclohexylbenzimidazole-5-carboxylate (87 g) obtained in Example 27 was dissolved in methyl alcohol (250 ml) and tetrahydrofuran (250 ml), and potassium carbonate (31 g) was added. The mixture was stirred for 30 min at room temperature. The insoluble materials were filtered off and the filtrate was concentrated under reduced pressure. Water was added to the residues and the mixture was neutralized with 2N hydrochloric acid. The precipitated crystals were collected by filtration to give the title compound (78 g, yield 97%).

후처리

  1. filtrationThe insoluble materials were filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionWater was added to the residues
  4. filtrationThe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-9079e15b77984d74b77eac367375ff65
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06770666B2

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