Benzene → HCID 19772346, 화합물

HRID 1614666노트

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HRID 1614666 반응식
[C:1]1([C:7]2[C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=3[CH2:10][S:9][C:8]=2C(O)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1C=CC(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:27])=CC=1.C1C=CC=CC=1.Cl.[C:44]([O:47][C:48]1[C:54]([CH3:55])=[CH:53][C:51]([NH2:52])=[CH:50][C:49]=1[CH3:56])(=[O:46])[CH3:45].C([N:59]([CH2:62]C)CC)C>>[C:44]([O:47][C:48]1[C:54]([CH3:55])=[CH:53][C:51]([NH:52][C:62]([NH:59][C:8]2[S:9][CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[C:7]=2[C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[O:27])=[CH:50][C:49]=1[CH3:56])(=[O:46])[CH3:45]

참가 물질

6

반응물 5

HCID 241BenzeneHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 19090525HCID 19090525, 화합물HCID 19090551HCID 19090551, 화합물

생성물 1

HCID 19772346HCID 19772346, 화합물

실험 절차

To a mixture of 4-phenyl-1H-2-benzothiopyran-3-carboxylic acid (in Reference Example 13) (268 mg), DPPA (330 mg) and benzene (5 ml) was added dropwise to triethylamime (0.14 ml) and the mixture was stirred at room temperature for 30 minutes, then refluxed for 30 minutes. To the mixture were added 4-acetoxy-3,5-dimethylaniline hydrochloride (258 mg) and triethylamine (0.17 ml), followed by refluxing for 20 minutes. The mixture was washed with water, then dried (MgSO4), followed by distilling off the solvent. To the residue was added ether to afford the above-titled compound as colorless crystals (280 mg).

후처리

  1. additionwas added dropwise to triethylamime (0.14 ml)
  2. temperaturerefluxed for 30 minutes
  3. temperatureby refluxing for 20 minutes
  4. washThe mixture was washed with water
  5. dry with materialdried (MgSO4)
  6. distillationby distilling off the solvent
  7. additionTo the residue was added ether

출처 및 근거

ORD 기록
ord-78d8a4ef24d14d13bf3b707abb7706da
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05198462

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