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 1615750ノート

反応式

HRID 1615750 の反応式
[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]

参加物

5

反応物 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

生成物 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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-761c3dd546b44a119b9dd6a8c0652b04
出典データセット
uspto-grants-2014_07
特許番号
US08765763B2

反応ノート

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