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Triethylamine → HCID 57565317, 화합물

HRID 1727042
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HRID 1727042 반응식
ClS(O)(=O)=O.[CH3:6][O:7][C:8](=[O:23])[CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([S:19](Cl)(=[O:21])=[O:20])[CH:16]=2)[CH2:11]1.[CH3:24][O:25][C:26](=[O:41])[CH2:27][CH:28]1[CH2:36][C:35]2[C:30](=[CH:31][CH:32]=[CH:33][C:34]=2[S:37](Cl)(=[O:39])=[O:38])[CH2:29]1.[F:42][C:43]([F:57])([F:56])[C:44]1[CH:49]=[CH:48][C:47]([N:50]2[CH2:55][CH2:54][NH:53][CH2:52][CH2:51]2)=[CH:46][CH:45]=1.C(N(CC)CC)C>C1COCC1.CN(C1C=CN=CC=1)C>[CH3:6][O:7][C:8](=[O:23])[CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([S:19]([N:53]3[CH2:52][CH2:51][N:50]([C:47]4[CH:46]=[CH:45][C:44]([C:43]([F:56])([F:57])[F:42])=[CH:49][CH:48]=4)[CH2:55][CH2:54]3)(=[O:21])=[O:20])[CH:16]=2)[CH2:11]1.[CH3:24][O:25][C:26](=[O:41])[CH2:27][CH:28]1[CH2:36][C:35]2[C:30](=[CH:31][CH:32]=[CH:33][C:34]=2[S:37]([N:53]2[CH2:52][CH2:51][N:50]([C:47]3[CH:46]=[CH:45][C:44]([C:43]([F:56])([F:57])[F:42])=[CH:49][CH:48]=3)[CH2:55][CH2:54]2)(=[O:39])=[O:38])[CH2:29]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 8471TriethylamineHCID 24638Chlorosulfonic acidHCID 1217181-(4-(Trifluoromethyl)phenyl)piperazineHCID 85864988HCID 85864988, 화합물HCID 86245824HCID 86245824, 화합물

생성물 2

HCID 57565317HCID 57565317, 화합물수율 19%
HCID 67046329
HCID 67046329, 화합물
수율 6%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

Indanyl-2-acetic acid methyl ester (1.0 g, 5.26 mmol) was added to a stirring solution of chlorosulfonic acid (5 mL) at 0° C. The solution was stirred at 0° C. for 0.5 h, then room temperature for 3 h. The resulting solution was poured slowly over ice and extracted with diethyl ether (3×100 mL). The combined organic layers were dried (Na2SO4) and concentrated to afford a mixture of 5-chlorosulfonyl-indan-2-acetic acid methyl ester and 4-chlorosulfonyl-indan-2-acetic acid methyl ester (1.38 g, 4.78 mmol. 91%). The sulfonyl chloride mixture was taken on to the next step without further purification. The mixture of sulfonyl chlorides (370 mg, 1.28 mmol) were dissolved in dry THF (10 mL). To this solution was added 1-(4-trifluoromethylphenyl)piperazine (315 mg, 1.37 mmol), triethylamine (600 μL, 4.3 mmol) and DMAP (catalytic amount). The reaction was stirred at room temperature for 1 h, concentrated and directly purified by silica gel flash column chromatography to separate the regioisomers (25% ethyl acetate in hexanes) affording {5-[4-(4-trifluoromethyl-phenyl)-piperazine-1-sulfonyl]-indan-2-yl}-acetic acid methyl ester (118 mg, 19%) and {4-[4-(4-trifluoromethyl-phenyl)-piperazine-1-sulfonyl]-indan-2-yl}-acetic acid methyl ester (40 mg, 6%) as clear colorless oils. {5-[4-(4-trifluoromethyl-phenyl)-piperazine-1-sulfonyl]-indan-2-yl}-acetic acid methyl ester: 1H NMR (400 MHz, CDCl3) 7.57 (s, 1H), 7.56 (d, 1H), 7.45 (d, 2H), 7.33 (d, 1H), 6.87 (d, 2H), 3.69 (s, 3H), 3.33 (m, 4H), 3.21 (dd, 2H), 3.14 (m, 4H), 2.95 (m, 1H), 2.71 (dd, 2H), 2.52 (d, 2H).

후처리

  1. waitroom temperature for 3 h
  2. additionThe resulting solution was poured slowly over ice
  3. extractionextracted with diethyl ether (3×100 mL)
  4. dry with materialThe combined organic layers were dried (Na2SO4)
  5. concentrationconcentrated
  6. customto afford
  7. customThe sulfonyl chloride mixture was taken on to the next step without further purification
  8. stirringThe reaction was stirred at room temperature for 1 h
  9. concentrationconcentrated
  10. customdirectly purified by silica gel flash column chromatography
  11. customto separate the regioisomers (25% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-6a57927609b24295b2a0883c226ef1a1
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07494999B2

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