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Propylamine → Propyl pentanesulfonamide

HRID 902219
ノート
印刷プレビュー

反応式

HRID 902219 の反応式
[CH2:1]([S:6](Cl)(=[O:8])=[O:7])[CH2:2][CH2:3][CH2:4][CH3:5].[CH2:10](N)[CH2:11][CH3:12].C([N:16](C(C)C)C(C)C)C>C(Cl)Cl>[CH2:10]([CH:1]([S:6]([NH2:16])(=[O:8])=[O:7])[CH2:2][CH2:3][CH2:4][CH3:5])[CH2:11][CH3:12]
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 7852PropylamineHCID 81531DiisopropylethylamineHCID 2375551-Pentanesulfonyl chloride

生成物 1

HCID 22322638Propyl pentanesulfonamide収率 95%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

Pentane sulfonyl chloride (687 mg, 4.03 mmol) was dissolved in 5 mL CH2Cl2 and added to an ice-cooled solution of n-propylamine (0.40 mL, 4.82 mmol) and ethyldiisopropylamine (0.85 mL, 4.88 mmol) in 5 mL CH2Cl2 under a nitrogen atmosphere. The reaction was stirred at 0° C. for 30 min, then at 25° C. for 4 h. The solution was partitioned between 20 mL of 1.0 M aqeous NaHSO4 and 25 mL CH2Cl2. The organic phase was washed sequentially with 25 mL H2O and 25 mL brine, then dried (Na2SO4), filtered, and concentrated in vacuo to provide 739 mg (3.83 mmol, 95%) of the title compound as a white solid. TLC (25% EtOAc-hexane) Rf 0.23; 1H NMR (CDCl3, 300 MHz) δ 0.92 (t, J=7 Hz, 3H), 0.97 (t, J=7 Hz, 3H), 1.28-1.50 (br m, 4H), 1.52-1.68 (m, 2H), 1.75-1.90 (br m, 2H), 2.98-3.06 (m, 2H), 3.08 (q, J=6 Hz, 2H), 4.10-4.23 (br m, 1H); MS (DCl/NH3) m/e 211 (M+NH4)+.

後処理

  1. waitat 25° C. for 4 h
  2. customThe solution was partitioned between 20 mL of 1.0 M aqeous NaHSO4 and 25 mL CH2Cl2
  3. washThe organic phase was washed sequentially with 25 mL H2O and 25 mL brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-0f6d4942946042ccb0c4e807977c8f66
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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