Methanol → HCID 59397939、化合物

HRID 39856ノート

反応式

HRID 39856 の反応式
CO.[C:3]([O:7][C:8]([N:10]([CH2:38][C:39]1[CH:48]=[CH:47][C:42]2[O:43][CH2:44][CH2:45][O:46][C:41]=2[CH:40]=1)[CH:11]1[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][N:19]2[C:28]3[C:23](=[CH:24][CH:25]=[C:26]([C:29]([O:31]CCCC)=[O:30])[CH:27]=3)[C:22]([CH3:36])=[CH:21][C:20]2=[O:37])[CH2:13][CH2:12]1)=[O:9])([CH3:6])([CH3:5])[CH3:4].O.[OH-].[Li+]>O>[C:3]([O:7][C:8]([N:10]([CH2:38][C:39]1[CH:48]=[CH:47][C:42]2[O:43][CH2:44][CH2:45][O:46][C:41]=2[CH:40]=1)[CH:11]1[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][N:19]2[C:28]3[C:23](=[CH:24][CH:25]=[C:26]([C:29]([OH:31])=[O:30])[CH:27]=3)[C:22]([CH3:36])=[CH:21][C:20]2=[O:37])[CH2:15][CH2:16]1)=[O:9])([CH3:4])([CH3:5])[CH3:6]

参加物

5

反応物 3

HCID 887MethanolHCID 168937Lithium hydroxide, monohydrate2 回HCID 59398232HCID 59398232、化合物

生成物 1

HCID 59397939HCID 59397939、化合物収率 101.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 11 mL of a methanol solution containing 0.65 g of butyl 1-(2-(4-((tert-butoxycarbonyl) (2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-4-methyl-2-oxo-1,2-dihydroquinoline-7-carboxylate, 55 mg of lithium hydroxide monohydrate was added and stirred for 30 min. Then, 55 mg of lithium hydroxide monohydrate and 1.1 mL of water were added and stirred for 2 hours. The methanol was removed under reduced pressure, water and chloroform were added, and adjusted to pH 5.0 with acetic acid. The organic layer was separated, and the aqueous layer was extracted with chloroform. The organic layer and extracts were combined, washed with aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to give 0.60 g of 1-(2-(4-((tert-butoxycarbonyl)(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-4-methyl-2-oxo-1,2-dihydroquinoline-7-carboxylic acid as a white foam.

後処理

  1. additionwas added
  2. stirringstirred for 2 hours
  3. customThe methanol was removed under reduced pressure, water and chloroform
  4. additionwere added
  5. customThe organic layer was separated
  6. extractionthe aqueous layer was extracted with chloroform
  7. washwashed with aqueous saturated sodium chloride solution
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-17d90650ebad4c788968c7ee39412a28
出典データセット
uspto-grants-2013_09
特許番号
US08524738B2

反応ノート

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