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Ammonia → 2-Trimethylsilanylethyl 4-((s)-1-tert-butoxycarbonylamino-1-methoxycarbonyl-but-3-enyl)piperidine-1-carboxylate

HRID 1743262
ノート
印刷プレビュー

反応式

HRID 1743262 の反応式
N.[Na].[CH2:3]([C@:6]1([CH:32]2[CH2:37][CH2:36][N:35]([C:38]([O:40][CH2:41][CH2:42][Si:43]([CH3:46])([CH3:45])[CH3:44])=[O:39])[CH2:34][CH2:33]2)[C:11](=[O:12])[O:10][C@@H:9](C2C=CC=CC=2)[C@@H](C2C=CC=CC=2)[N:7]1[C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH:4]=[CH2:5].[Cl-].[NH4+].C[Si](C=[N+]=[N-])(C)C>C1COCC1.CO.CCCCCC.C(O)(=O)C.C(O)C>[C:28]([O:27][C:25]([NH:7][C@@:6]([CH:32]1[CH2:37][CH2:36][N:35]([C:38]([O:40][CH2:41][CH2:42][Si:43]([CH3:46])([CH3:45])[CH3:44])=[O:39])[CH2:34][CH2:33]1)([C:11]([O:10][CH3:9])=[O:12])[CH2:3][CH:4]=[CH2:5])=[O:26])([CH3:29])([CH3:30])[CH3:31]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

HCID 222Ammonia2 回HCID 25517Ammonium ChlorideHCID 167693TrimethylsilyldiazomethaneHCID 5360545SodiumHCID 90954080Tert-butyl (3s,5r,6s)-3-allyl-2-oxo-5,6-diphenyl-3-[1-(2-trimethylsilanylethoxycarbonyl)piperidin-4-yl]morpholine-4-carboxylate

生成物 1

HCID 69651597
2-Trimethylsilanylethyl 4-((s)-1-tert-butoxycarbonylamino-1-methoxycarbonyl-but-3-enyl)piperidine-1-carboxylate

試薬・触媒・溶媒 5

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 8058Hexane溶媒

反応条件

温度
0 °C

実験手順

50 ml of ammonia were condensed at −78° C. 340 mg of sodium were added in 2 portions at an interval of 10 min in each case and the mixture was stirred for 20 min. At −60° C., a solution of 916 mg of tert-butyl (3S,5R,6S)-3-allyl-2-oxo-5,6-diphenyl-3-[1-(2-trimethylsilanylethoxycarbonyl)piperidin-4-yl]morpholine-4-carboxylate and 866 μl of ethanol in 50 ml of THF was added dropwise. The mixture was stirred at −45° C. for 1.5 h, and the reaction was stopped by adding solid ammonium chloride until the blue color disappeared. The ammonia was then allowed to evaporate off, and 150 ml of water were added to the residue. The THF was removed in vacuo. The aqueous was adjusted to pH 2 with 1 N HCl and extracted 3 times with 100 ml of ethyl acetate each time. The combined organic phases were dried with MgSO4. The solvents were removed in vacuo, and the residue was filtered through silica gel with 4% methanol in dichloromethane. The product obtained in this way was taken up in 5 ml of methanol and cooled to 0° C. 0.5 ml of a 2 N solution of trimethylsilyldiazomethane in hexane was added thereto 5 times at intervals of 1.5 hours each. 2 ml of acetic acid were then added dropwise, and the mixture was stirred at room temperature for 1 h. The solvents were removed in vacuo and the residue was chromatographed on silica gel.

後処理

  1. customcondensed at −78° C
  2. stirringThe mixture was stirred at −45° C. for 1.5 h
  3. customto evaporate off
  4. addition150 ml of water were added to the residue
  5. customThe THF was removed in vacuo
  6. extractionextracted 3 times with 100 ml of ethyl acetate each time
  7. dry with materialThe combined organic phases were dried with MgSO4
  8. customThe solvents were removed in vacuo
  9. filtrationthe residue was filtered through silica gel with 4% methanol in dichloromethane
  10. customThe product obtained in this way
  11. customat intervals of 1.5 hours
  12. stirringthe mixture was stirred at room temperature for 1 h
  13. customThe solvents were removed in vacuo
  14. customthe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-58e5eb2983b245cca925f02d1f121d3d
出典データセット
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07008957B2

反応ノート

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