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Triethylamine → N-(3-pyridylmethyl)-5-chloro-3-phenylthioindole-2-carboxamide

HRID 260460
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HRID 260460 반응식
F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.[Cl:28][C:29]1[CH:30]=[C:31]2[C:35](=[CH:36][CH:37]=1)[NH:34][C:33]([C:38](O)=[S:39])=[C:32]2[C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1.[NH2:47][CH2:48][C:49]1[CH:50]=[N:51][CH:52]=[CH:53][CH:54]=1.C(N(CC)CC)C>CN(C)C=O>[N:51]1[CH:52]=[CH:53][CH:54]=[C:49]([CH2:48][NH:47][C:38]([C:33]2[NH:34][C:35]3[C:31]([C:32]=2[C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)=[CH:30][C:29]([Cl:28])=[CH:37][CH:36]=3)=[S:39])[CH:50]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 310183-PyridinemethanamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 178526153HCID 178526153, 화합물

생성물 1

HCID 86749574N-(3-pyridylmethyl)-5-chloro-3-phenylthioindole-2-carboxamide

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

Benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorphosphate (0.73 g, 1.6 mmol) was added to a solution of 5-chloro-3-phenylthio-indole-2-carboxylic acid (0.50 g, 1.6 mmol), 3-aminomethylpyridine (0.35 g, 3.2 mmol) and triethylamine (0.50 mL, 3.2 mmol) in degassed dimethylformamide (25 mL). The reaction was stirred at room temperature overnight. The precipitated product was filtered and the filter cake washed well with water. The solid was triturated with 30% ethyl acetate in hexane, filtered and dried at 60° C. in vacuo for 72 h. The title compound was obtained as an off-white solid, mp 240°-241° C. Anal. Calc. for C21H16ClN3OS.0.25 H2O: C, 63.31; H, 4.17; N, 10.54. Found: C, 63.34; H, 4.06; N, 10.71. NMR (DMSO-d6): δ12.54 (1H, s), 8.91 (1H, t, J=6 Hz), 8.51 (1H, s), 8.42 (1H, d, J=5 Hz), 7.58 (2H, m), 7.45 (1H, m), 7.25 (4H, m), 7.15 (1H, t, J=7 Hz), 7.04 (2H, d, J=8 Hz), 4.58 (2H, d, J=6 Hz).

후처리

  1. filtrationThe precipitated product was filtered
  2. washthe filter cake washed well with water
  3. customThe solid was triturated with 30% ethyl acetate in hexane
  4. filtrationfiltered
  5. customdried at 60° C. in vacuo for 72 h

출처 및 근거

ORD 기록
ord-5d27dcdc32c1461fa49b63fa50397c40
출처 데이터셋
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05527819

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