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Trifluoromethanesulfonic anhydride → [4-[2-[Bis-(isopropyl)-amino]-2-oxoethoxy]-2,3-dicyanophenyl]trifluoromethanesulfonate

HRID 400248
ノート
印刷プレビュー

反応式

HRID 400248 の反応式
C(N(C(C)C)C(C)C)C.[F:10][C:11]([F:24])([F:23])[S:12]([O:15]S(C(F)(F)F)(=O)=O)(=[O:14])=[O:13].[CH:25]([N:28]([CH:44]([CH3:46])[CH3:45])[C:29](=[O:43])[CH2:30][O:31][C:32]1[CH:37]=[CH:36][C:35](O)=[C:34]([C:39]#[N:40])[C:33]=1[C:41]#[N:42])([CH3:27])[CH3:26]>C(#N)C>[CH:44]([N:28]([CH:25]([CH3:27])[CH3:26])[C:29](=[O:43])[CH2:30][O:31][C:32]1[CH:37]=[CH:36][C:35]([O:15][S:12]([C:11]([F:24])([F:23])[F:10])(=[O:14])=[O:13])=[C:34]([C:39]#[N:40])[C:33]=1[C:41]#[N:42])([CH3:46])[CH3:45]
参加物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 67749Trifluoromethanesulfonic anhydrideHCID 81531DiisopropylethylamineHCID 21841501N,N-bis-(isopropyl)-2-(2,3-dicyano-4-hydroxy-phenoxy)-acetamide

生成物 1

HCID 21841500[4-[2-[Bis-(isopropyl)-amino]-2-oxoethoxy]-2,3-dicyanophenyl]trifluoromethanesulfonate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

0.58 ml of ethyl diisopropylamine and 0.59 ml of trifluoromethanesulfonic anhydride were added to a solution of 900 mg of the product of Stage A in 50 ml of acetonitrile and the reaction medium was refluxed for one hour. Then, the solvent was evaporated under reduced pressure and the crude product obtained was chromatographed on silica, eluting with a cyclohexane-ethyl acetate mixture (50-50) to obtain 600 mg of the expected product.

後処理

  1. temperaturethe reaction medium was refluxed for one hour
  2. customThen, the solvent was evaporated under reduced pressure
  3. customthe crude product obtained
  4. customwas chromatographed on silica
  5. washeluting with a cyclohexane-ethyl acetate mixture (50-50)

出典と根拠

ORDレコード
ord-c3fac434a22744048a6562508ca1523d
出典データセット
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05827887

反応ノート

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