Lithium Hydroxide → (R)-2-(1-(tert-butoxycarbonyl)-5-oxo-3-phenyl-8,11-dioxa-1,4-diazaspiro[5.6]dodecan-4-yl)ethanoic acid

HRID 1615750노트

반응식

HRID 1615750 반응식
[OH-].[Li+].C[O:4][C:5](=[O:33])[CH2:6][N:7]1[C:12](=[O:13])[C:11]2([CH2:19][O:18][CH2:17][CH2:16][O:15][CH2:14]2)[N:10]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:9][C@H:8]1[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1>O.CO>[C:23]([O:22][C:20]([N:10]1[C:11]2([CH2:19][O:18][CH2:17][CH2:16][O:15][CH2:14]2)[C:12](=[O:13])[N:7]([CH2:6][C:5]([OH:33])=[O:4])[C@H:8]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH2:9]1)=[O:21])([CH3:26])([CH3:24])[CH3:25]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 68154106(R)-tert-butyl 4-(2-methoxy-2-oxoethyl)-5-oxo-3-phenyl-8,11-dioxa-1,4-diazaspiro[5.6]dodecane-1-carboxylate

생성물 1

HCID 68154418(R)-2-(1-(tert-butoxycarbonyl)-5-oxo-3-phenyl-8,11-dioxa-1,4-diazaspiro[5.6]dodecan-4-yl)ethanoic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

24 mg (1.0 mmol) lithium hydroxide in 1 ml of water were added to 0.22 g (0.5 mmol) (R)-tert-butyl 4-(2-methoxy-2-oxoethyl)-5-oxo-3-phenyl-8,11-dioxa-1,4-diazaspiro[5.6]dodecane-1-carboxylate in 10 ml MeOH. The reaction mixture was stirred overnight at RT and then the MeOH was distilled off. The residue was mixed with water and acidified with an aqueous 4N hydrochloric acid. The aqueous phase was extracted with ethyl acetate. The ethyl acetate phase was dried and evaporated down.

후처리

  1. distillationthe MeOH was distilled off
  2. additionThe residue was mixed with water
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. dry with materialThe ethyl acetate phase was dried
  5. customevaporated down

출처 및 근거

ORD 기록
ord-761c3dd546b44a119b9dd6a8c0652b04
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765763B2

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