Water → (R)-tert-butyl 3-(N-methylcyclopropanesulfonamido)pyrrolidine-1-carboxylate

HRID 527909ノート

反応式

HRID 527909 の反応式
[CH3:1][NH:2][C@@H:3]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4]1.[CH:15]1([S:18](Cl)(=[O:20])=[O:19])[CH2:17][CH2:16]1.CCN(C(C)C)C(C)C.O>C1COCC1>[CH3:1][N:2]([C@@H:3]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4]1)[S:18]([CH:15]1[CH2:17][CH2:16]1)(=[O:20])=[O:19]

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 2760919Cyclopropanesulfonyl chlorideHCID 45089543tert-butyl (3R)-3-(methylamino)pyrrolidine-1-carboxylate

生成物 1

HCID 86692139(R)-tert-butyl 3-(N-methylcyclopropanesulfonamido)pyrrolidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (R)-tert-butyl 3-(methylamino)pyrrolidine-1-carboxylate (100 mg, 0.5 mmol) in 2.5 mL THF was added cyclopropanesulfonyl chloride (77 mg, 0.55 mmol) and DIPEA (0.10 mL, 0.60 mmol) at ambient temperature. The mixture was stirred at ambient temperature overnight. Water was added, and then extracted with EtOAc. The organic layers were combined washed with brine, dried over Na2SO4, and evaporated in vacuo to afford the crude title product which was used for the next step without further purification. MS (m/z): 305 (M+H)+.

後処理

  1. extractionextracted with EtOAc
  2. washThe organic layers were combined washed with brine
  3. dry with materialdried over Na2SO4
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-0986bf05a58746b7902fd350e99fefc6
出典データセット
uspto-grants-2016_05
特許番号
US09346810B2

反応ノート

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