Sodium Hydroxide → HCID 21043774, 화합물

HRID 11871노트

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HRID 11871 반응식
C[O:2][C:3](=[O:47])[C@H:4]([C:23](=[O:46])[C:24]1[CH:29]=[CH:28][C:27]([CH2:30][N:31]([C:39]([O:41][C:42]([CH3:45])([CH3:44])[CH3:43])=[O:40])[CH2:32][C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][N:34]=2)=[CH:26][CH:25]=1)[CH2:5][CH2:6][CH2:7][N:8]([CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=1)[C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10].[OH-].[Na+]>CO>[C:39]([N:31]([CH2:30][C:27]1[CH:28]=[CH:29][C:24]([C:23]([C@H:4]([CH2:5][CH2:6][CH2:7][N:8]([CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=2)[C:9]([O:11][C:12]([CH3:15])([CH3:13])[CH3:14])=[O:10])[C:3]([OH:47])=[O:2])=[O:46])=[CH:25][CH:26]=1)[CH2:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][N:34]=1)([O:41][C:42]([CH3:43])([CH3:44])[CH3:45])=[O:40]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 69638119(S)-2-(4-(N-Boc-N-(2-picolyl)aminomethyl)benzoyl)-5-(N-Boc-2-picolylamino)valeric acid methyl ester

생성물 1

HCID 21043774HCID 21043774, 화합물수율 91.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The compound obtained in Example 66-3 (8.96 g) was dissolved in methanol (134.4 ml) and 1 N aqueous solution of sodium hydroxide (134.4 ml) was added. The mixture was stirred for 1 day. After confirming completion of the reaction with TLC, the reaction solution was concentrated under reduced pressure. The residue was dissolved in 1N aqueous solution of sodium hydroxide and washed with diisopropyl ether. 1 N hydrochloric acid aqueous solution was added to the resulting water layer to adjust the pH to 2-3. The solution was extracted with ethyl acetate and the organic layer separated was dried over anhydrous sodium sulfate, concentrated under reduced pressure, and dried under vacuum to obtain the title compound (8.04 g) as a light brown solid.

후처리

  1. customcompletion of the reaction with TLC
  2. concentrationthe reaction solution was concentrated under reduced pressure
  3. dissolutionThe residue was dissolved in 1N aqueous solution of sodium hydroxide
  4. washwashed with diisopropyl ether
  5. addition1 N hydrochloric acid aqueous solution was added to the resulting water layer
  6. extractionThe solution was extracted with ethyl acetate
  7. customthe organic layer separated
  8. dry with materialwas dried over anhydrous sodium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customdried under vacuum

출처 및 근거

ORD 기록
ord-12f48c0cf7f24a37988025d4c331fd79
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098215B2

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