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Sodium hydride → HCID 44315917、化合物

HRID 1656469
ノート
印刷プレビュー

反応式

HRID 1656469 の反応式
[CH3:1][CH:2]([S:16]([NH2:19])(=[O:18])=[O:17])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15].[H-].[Na+].[CH:22]([C:25]1[CH:30]=[CH:29][CH:28]=[C:27]([CH:31]([CH3:33])[CH3:32])[C:26]=1[N:34]=[C:35]=[O:36])([CH3:24])[CH3:23]>CN(C=O)C>[CH3:24][CH:22]([C:25]1[CH:30]=[CH:29][CH:28]=[C:27]([CH:31]([CH3:32])[CH3:33])[C:26]=1[NH:34][C:35]([NH:19][S:16]([CH:2]([CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])[CH3:1])(=[O:18])=[O:17])=[O:36])[CH3:23]
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 922592,6-Diisopropylphenyl isocyanateHCID 21225990HCID 21225990、化合物

生成物 1

HCID 44315917HCID 44315917、化合物収率 60.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

反応条件

温度
0 °C

実験手順

A solution of 2-pentadecylsulfonamide (2.91 g, 10 mmoles) in DMF (40 mL dried over 3 Å sieves) was added dropwise to a stirred, 0° C. suspension of NaH (0.5 g, 21 mmoles of hexane washed) in 10 mL dry DMF. The mixture was stirred 30 minutes at 0° C., then warmed to room temperature for 3 hours. It was then cooled back to 0° C. and a solution of 2,6-diisopropylphenylisocyanate (2.14 mL, 10 mmoles) in 10 mL DMF was added dropwise. The mixture was allowed to warm to room temperature overnight, cooled to 0° C., and quenched by dropwise addition of 1N HCl (60 mL). The mixture was partitioned between EtOAc (300 mL) and H2O (100 mL). The organic layer was further washed with brine, dried, filtered, and evaporated to provide an oil which was flash chromatographed (silica gel, 4:1 hexane-EtOAc) to produce 3 g of an oil which solidified on standing (m.p. 65°-75° C.).

後処理

  1. temperaturewarmed to room temperature for 3 hours
  2. temperatureIt was then cooled back to 0° C.
  3. temperatureto warm to room temperature overnight
  4. temperaturecooled to 0° C.
  5. customquenched by dropwise addition of 1N HCl (60 mL)
  6. customThe mixture was partitioned between EtOAc (300 mL) and H2O (100 mL)
  7. washThe organic layer was further washed with brine
  8. customdried
  9. filtrationfiltered
  10. customevaporated
  11. customto provide an oil which
  12. customchromatographed (silica gel, 4:1 hexane-EtOAc)

出典と根拠

ORDレコード
ord-35a33621d7b64952b24bea5877322456
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05254589

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート