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Sodium hydride → N-Boc-N-propyl-O-allylhydroxylamine

HRID 902230
ノート
印刷プレビュー

反応式

HRID 902230 の反応式
[C:1]([NH:8][O:9][CH2:10][CH:11]=[CH2:12])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[H-].[Na+].I[CH2:16][CH2:17][CH3:18]>C1COCC1>[C:1]([N:8]([CH2:16][CH2:17][CH3:18])[O:9][CH2:10][CH:11]=[CH2:12])([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2]
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

5

反応物 3

HCID 24758Sodium hydrideHCID 336431-IodopropaneHCID 22322878Carbamic acid, (2-propenyloxy)-, 1,1-dimethylethyl ester (9CI)

生成物 1

HCID 22322817N-Boc-N-propyl-O-allylhydroxylamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

N-Boc-O-allylhydroxylamine (6.5 g) from the above procedure was dissolved in dry THF (25 mL) and the solution cooled to 0° C. in an ice bath. Sodium hydride (1.5 g, 60% dispersion in oil) was added portionwise over 5 min. The resulting mixture was stirred for 30 min at 0° C. 1-Iodopropane (3.8 mL) was added dropwise to the mixture. The reaction was stirred at 0° C. for 1 hour, then stirred overnight at room temperature. The THF was removed in vacuo and the residue taken up in EtOAc (50 mL) and washed with water (1×50 mL), saturated sodium bicarbonate solution (3×50 mL),1N phosphoric acid (3×50 mL), and brine (1×50 mL). The organic layer was dried with sodium sulfate and evaporated to give a light yellow oil, which was purified by flash chromatography on silica gel eluting with 5% EtOAc/hexanes to give the title compound as a colorless oil (6.0 g).

後処理

  1. stirringThe reaction was stirred at 0° C. for 1 hour
  2. stirringstirred overnight at room temperature
  3. customThe THF was removed in vacuo
  4. washwashed with water (1×50 mL), saturated sodium bicarbonate solution (3×50 mL),1N phosphoric acid (3×50 mL), and brine (1×50 mL)
  5. dry with materialThe organic layer was dried with sodium sulfate
  6. customevaporated
  7. customto give a light yellow oil, which
  8. customwas purified by flash chromatography on silica gel eluting with 5% EtOAc/hexanes

出典と根拠

ORDレコード
ord-9f24895f0c5b45ffbd55167a1c694d26
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07365093B2

反応ノート

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