Methanol → HCID 59397939, 화합물

HRID 2193229노트

반응식

HRID 2193229 반응식
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]

참가 물질

5

반응물 3

HCID 887MethanolHCID 168937Lithium hydroxide, monohydrate2회HCID 59398232HCID 59398232, 화합물

생성물 1

HCID 59397939HCID 59397939, 화합물수율 101.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a5f092785a2c4120ac3ed6612351576b
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329694B2

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