Hydrochloric Acid → HCID 59454486、化合物

HRID 455247ノート

反応式

HRID 455247 の反応式
[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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 86644710HCID 86644710、化合物

生成物 1

HCID 59454486HCID 59454486、化合物収率 83%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-4acb2157147846b680401152743f5c3d
出典データセット
uspto-grants-2013_07
特許番号
US08497274B2

反応ノート

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