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Acetic Acid → (3S,4S)-4-[(1R)-2-{(2S,4S)-1-allyloxycarbonyl-2-(2-fluoroethyloxymethyl)pyrrolidin-4-yl-thio}-1-methyl-2-oxoethyl]-3-{(1R)-1-(t-butyldimethylsilyl-oxy)ethyl}-2-azetidinone

HRID 703590
ノート
印刷プレビュー

反応式

HRID 703590 の反応式
[Si:1]([O:8][C@@H:9]([C@@H:11]1[C@@H:14]([C@@H:15]([CH3:24])[C:16](=[O:23])N2CCSC2=S)[NH:13][C:12]1=[O:25])[CH3:10])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[CH2:26]([O:29][C:30]([N:32]1[CH2:36][CH:35]([SH:37])[CH2:34][CH:33]1[CH2:38][O:39][CH2:40][CH2:41][F:42])=[O:31])[CH:27]=[CH2:28].C(N(CC)CC)C.C(O)(=O)C>O1CCCC1>[CH2:26]([O:29][C:30]([N:32]1[CH2:36][C@@H:35]([S:37][C:16](=[O:23])[C@@H:15]([C@H:14]2[NH:13][C:12](=[O:25])[C@@H:11]2[C@H:9]([O:8][Si:1]([C:4]([CH3:5])([CH3:6])[CH3:7])([CH3:2])[CH3:3])[CH3:10])[CH3:24])[CH2:34][C@H:33]1[CH2:38][O:39][CH2:40][CH2:41][F:42])=[O:31])[CH:27]=[CH2:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 8471TriethylamineHCID 14071070(3S,4R)-3-[(1R)-1-(t-butyldimethylsilyloxy)ethyl]-4-{(1R)-1-methyl-2-oxo-2-(2-thioxothiazolidin-3-yl)ethyl]-2-azetidinoneHCID 190870681-Allyloxycarbonyl-2-(2-fluoroethyloxymethyl)-4-mercaptopyrrolidine

生成物 1

HCID 86744487
(3S,4S)-4-[(1R)-2-{(2S,4S)-1-allyloxycarbonyl-2-(2-fluoroethyloxymethyl)pyrrolidin-4-yl-thio}-1-methyl-2-oxoethyl]-3-{(1R)-1-(t-butyldimethylsilyl-oxy)ethyl}-2-azetidinone
収率 42.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (3S,4R)-3-[(1R)-1-(t-butyldimethylsilyloxy)ethyl]- 4-{(1R)-1-methyl-2-oxo-2-(2-thioxothiazolidin-3-yl)ethyl]-2-azetidinone (3.17 g) in tetrahydrofuran (30 ml) were added 1-allyloxycarbonyl-2-(2-fluoroethyloxymethyl)-4-mercaptopyrrolidine (2.21 g) and triethylamine (1.46 ml) at 5° C., and the mixture was stirred at room temperature for 8.5 hours. Acetic acid (0.63 ml) was added to the mixture and the mixture was evaporated. The residue was dissolved in water and ethyl acetate. The organic layer was separated, washed with water, dried and evaporated. The residue was purified by chromatography on silica gel eluting with a mixture of dichloromethane and ethyl acetate (2:1 V/V) to give (3S,4S)-4-[(1R)-2-{(2S,4S)-1-allyloxycarbonyl-2-(2-fluoroethyloxymethyl)pyrrolidin-4-yl-thio}-1-methyl-2-oxoethyl]-3-{(1R)-1-(t-butyldimethylsilyl-oxy)ethyl}-2-azetidinone (1.82 g).

後処理

  1. customthe mixture was evaporated
  2. dissolutionThe residue was dissolved in water
  3. customThe organic layer was separated
  4. washwashed with water
  5. customdried
  6. customevaporated
  7. customThe residue was purified by chromatography on silica gel eluting with a mixture of dichloromethane and ethyl acetate (2:1 V/V)

出典と根拠

ORDレコード
ord-6c308863892e4e06947e8d7c752d0899
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04983596

反応ノート

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