tert-Butanol → HCID 54493274, 화합물

HRID 1779431노트

반응식

HRID 1779431 반응식
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

참가 물질

5

반응물 4

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

생성물 1

HCID 54493274HCID 54493274, 화합물

실험 절차

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)).

후처리

  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))

출처 및 근거

ORD 기록
ord-1a12e22b73b24525b9999861d79ae096
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05627198

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