tert-Butanol → HCID 54493274、化合物

HRID 1779431ノート

反応式

HRID 1779431 の反応式
C([N:3]([CH2:6][CH3:7])[CH2:4]C)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:15])C=CC=CC=1.[C:25]1([S:31]([C:34]2[S:38]C(C(O)=O)=C[CH:35]=2)(=[O:33])=[O:32])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.[C:42]([OH:46])([CH3:45])([CH3:44])[CH3:43]>>[C:25]1([S:31]([C:34]2[S:38][C:6]([NH:3][C:4](=[O:15])[O:46][C:42]([CH3:45])([CH3:44])[CH3:43])=[CH:7][CH:35]=2)(=[O:32])=[O:33])[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1

参加物

5

反応物 4

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 2202575-(Benzenesulfonyl)thiophene-2-carboxylic acid

生成物 1

HCID 54493274HCID 54493274、化合物

実験手順

Triethylamine (0.62 ml, 4.4 mmol) and diphenylphosphoryl azide (0.97 ml, 4.5 mmol) are added to 5-(phenylsulfonyl)thiophene-2-carboxylic acid (1.00 g, 3.7 mmol) in 40 ml of absolute tert-butanol. The reaction mixture is boiled under reflux for 5 hours. The solvent is distilled off. The residue is taken up in ethyl acetate and washed with water. The organic phase is dried over magnesium sulfate and filtered and the solvent is distilled off. The green-black oil which remains is purified by flash chromatography (eluent: 33% v/v ethyl acetate in petroleum ether (40/60)).

後処理

  1. temperatureunder reflux for 5 hours
  2. distillationThe solvent is distilled off
  3. washwashed with water
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. distillationthe solvent is distilled off
  7. customThe green-black oil which remains is purified by flash chromatography (eluent: 33% v/v ethyl acetate in petroleum ether (40/60))

出典と根拠

ORDレコード
ord-1a12e22b73b24525b9999861d79ae096
出典データセット
uspto-grants-1997_05
特許番号
US05627198

反応ノート

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