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Hydrochloric Acid → HCID 178506082、化合物

HRID 1497236
ノート
印刷プレビュー

反応式

HRID 1497236 の反応式
Cl[C:2]1[C:11]([C:12]2[NH:16][N:15]=[N:14][N:13]=2)=[C:10]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:23]([F:26])([F:25])[F:24])[CH:8]=2)[N:3]=1.[NH:27]1[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]1.C(N(CC)CC)C.Cl>CC(N(C)C)=O>[C:17]1([C:10]2[C:9]3[C:4](=[CH:5][CH:6]=[C:7]([C:23]([F:26])([F:25])[F:24])[CH:8]=3)[N:3]=[C:2]([N:27]3[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]3)[C:11]=2[C:12]2[NH:16][N:15]=[N:14][N:13]=2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8082PiperidineHCID 8471TriethylamineHCID 178506080HCID 178506080、化合物

生成物 1

HCID 178506082HCID 178506082、化合物収率 18.6%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2-chloro-4-phenyl-3-(1H-tetrazol-5-yl)-6-trifluoromethyl-quinoline (105 mg, 279 μmol), piperidine (47.6 mg, 55.3 μl, 559 μmol) and triethylamine (84.8 mg, 117 μl, 838 μmol) in DMA (2 ml) was heated to 100° C. in a sealed tube. After 4 h 0.1N HCl was added at room temperature and the mixture was extracted with EtOAc. The combined organic layers were washed with 0.1N HCl and brine and dried with Na2SO4. The remaining brown oil was purified by chromatography (silica gel, DCM/MeOH 98:2 to 95:5). The product fractions were concentrated and the remaining solid was dissolved in EtOAc, filtered through silica gel and evaporated. The remaining residue was finally purified by preparative thin-layer chromatography (DCM/MeOH 95:5) to obtain the title compound (22 mg, 18%) as light yellow solid. MS (ESI): 425.4 (M+H)+.

後処理

  1. extractionthe mixture was extracted with EtOAc
  2. washThe combined organic layers were washed with 0.1N HCl and brine
  3. dry with materialdried with Na2SO4
  4. customThe remaining brown oil was purified by chromatography (silica gel, DCM/MeOH 98:2 to 95:5)
  5. concentrationThe product fractions were concentrated
  6. dissolutionthe remaining solid was dissolved in EtOAc
  7. filtrationfiltered through silica gel
  8. customevaporated
  9. customThe remaining residue was finally purified by preparative thin-layer chromatography (DCM/MeOH 95:5)

出典と根拠

ORDレコード
ord-94d7cee912bb44da9788857304709a7e
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09199938B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート