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Phenyl isocyanate → HCID 131720864, 화합물

HRID 399077
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HRID 399077 반응식
[CH3:1][C:2]1([CH3:23])[CH:5]([OH:6])[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[C:3]1[C:13]1[CH:18]=[CH:17][C:16]([S:19]([CH3:22])(=[O:21])=[O:20])=[CH:15][CH:14]=1.C(N(C(C)C)CC)(C)C.[C:33]1([N:39]=[C:40]=[O:41])[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1>C1(C)C=CC=CC=1.CCOC(C)=O.O>[CH3:1][C:2]1([CH3:23])[CH:5]([OH:6])[C:4]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[C:3]1[C:13]1[CH:14]=[CH:15][C:16]([S:19]([CH3:22])(=[O:21])=[O:20])=[CH:17][CH:18]=1.[C:33]1([NH:39][C:40](=[O:6])[O-:41])[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 7672Phenyl isocyanateHCID 81531DiisopropylethylamineHCID 18969768HCID 18969768, 화합물

생성물 1

HCID 131720864HCID 131720864, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 1140Toluene용매
HCID 8857
Ethyl Acetate
용매

실험 절차

To a solution of Example 62 (150 mg) in toluene (2.3 mL) at r.t., was added diisopropylethylamine (160 μL) and phenylisocyanate (100 μL ). The mixture was refluxed for 4 hr, cooled to r.t. and diluted with EtOAc and H2O. The organic phase was washed with HCl 1N, brine, dried (MgSO4) and the solvents evaporated. The residue was purified by flash chromatography (silica gel; hexane/EtOAc (80:20 to 60:40)) to give the title compound as a white solid, m.p. 85.5°-87° C.

후처리

  1. temperatureThe mixture was refluxed for 4 hr
  2. washThe organic phase was washed with HCl 1N, brine
  3. dry with materialdried (MgSO4)
  4. customthe solvents evaporated
  5. customThe residue was purified by flash chromatography (silica gel; hexane/EtOAc (80:20 to 60:40))

출처 및 근거

ORD 기록
ord-84d3d433a4ff414ebb385aed24447486
출처 데이터셋
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05817700

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