Hydrochloric Acid → HCID 59454486, 화합물

HRID 455247노트

반응식

HRID 455247 반응식
[CH:1]1([C:4]([NH:6][C:7]2[S:8][C:9]3[C:15]([C:16]([O:18]C)=[O:17])=[C:14]([O:20][C:21]4[CH:26]=[CH:25][C:24]([F:27])=[C:23]([NH:28][C:29](=[O:41])[CH2:30][C:31]5[CH:36]=[CH:35][CH:34]=[C:33]([C:37]([F:40])([F:39])[F:38])[CH:32]=5)[CH:22]=4)[CH:13]=[CH:12][C:10]=3[N:11]=2)=[O:5])[CH2:3][CH2:2]1.CO.O.[OH-].[Li+].Cl>O1CCCC1.O>[CH:1]1([C:4]([NH:6][C:7]2[S:8][C:9]3[C:15]([C:16]([OH:18])=[O:17])=[C:14]([O:20][C:21]4[CH:26]=[CH:25][C:24]([F:27])=[C:23]([NH:28][C:29](=[O:41])[CH2:30][C:31]5[CH:36]=[CH:35][CH:34]=[C:33]([C:37]([F:40])([F:39])[F:38])[CH:32]=5)[CH:22]=4)[CH:13]=[CH:12][C:10]=3[N:11]=2)=[O:5])[CH2:3][CH2:2]1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 86644710HCID 86644710, 화합물

생성물 1

HCID 59454486HCID 59454486, 화합물수율 83%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 2-[(cyclopropylcarbonyl)amino]-6-[4-fluoro-3-({[3-(trifluoromethyl)phenyl]acetyl}amino)phenoxy]-1,3-benzothiazole-7-carboxylate (1.50 g, 2.68 mmol) produced in Example 54(iv) in tetrahydrofuran (24 mL)/methanol (8 mL) was added a solution of lithium hydroxide monohydrate (1.05 g, 25.7 mmol) in water (8 mL), and the mixture was stirred at room temperature for 18 hr. The reaction mixture was neutralized with 1N hydrochloric acid, and the organic solvent was evaporated under reduced pressure. The obtained residue was collected by filtration, repeatedly washed with water to give the title compound (1.27 g, 83%) as a white powder.

후처리

  1. customthe organic solvent was evaporated under reduced pressure
  2. filtrationThe obtained residue was collected by filtration
  3. washrepeatedly washed with water

출처 및 근거

ORD 기록
ord-4acb2157147846b680401152743f5c3d
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08497274B2

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