Hydrochloric Acid → HCID 19037321、化合物

HRID 263383

反応式

HRID 263383 の反応式
[Cl:1][C:2]1[C:8]([O:9][CH:10]([CH3:12])[CH3:11])=[CH:7][C:5]([NH2:6])=[C:4]([F:13])[CH:3]=1.C[Al](C)C.[NH:18]1[CH2:28][CH2:27][CH2:26][CH2:25][CH:19]1[C:20](OCC)=[O:21].Cl>C(Cl)Cl.O>[Cl:1][C:2]1[C:8]([O:9][CH:10]([CH3:11])[CH3:12])=[CH:7][C:5]([NH:6][C:20]([CH:19]2[CH2:25][CH2:26][CH2:27][CH2:28][NH:18]2)=[O:21])=[C:4]([F:13])[CH:3]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 27517Ethyl piperidine-2-carboxylateHCID 158649Benzenamine, 4-chloro-2-fluoro-5-(1-methylethoxy)-HCID 16682925Trimethylaluminum

生成物 1

HCID 19037321HCID 19037321、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

The product of Example 1, Step A (4.25 g, 26.37 mmol) was dissolved in CH2Cl2 (200 mL). A solution of 2.0M trimethylaluminum (52.75 mmol) was added dropwise under nitrogen at 0° C. The resultant mixture was stirred at room temperature overnight. Ethyl pipecolinate (4.15 g) was added dropwise to the mixture and the mixture was stirred for 2 days. To the reaction mixture 6N HCl (100 mL) was added dropwise at 0° C. 200 mL of H2O was added, followed by the addition of 150 mL of methylene chloride. The aqueous layer was separated and basicified to pH 10 with 50% aqueous NaOH. 500 mL of CH2Cl2 was added. The organic layer was separated, dried over MgSO4, filtered and evaporated to dryness under vacuum to give the title compound of Step A as a white solid, 4.7 g. m.p. 96°-98° C. 1H NMR (CDCl3): δ9.25 (br s,1H), 8.17 (d,1H), 7.13 (d,1H) 4.58 (m,1H), 3.20 (M,1H), 3.10 (m,1H), 2.79 (m,1H), 2.00 (m,1H), 1.89 (m,2H), 1.60-1.40 (m,4H), 1.36 (d,6H).

後処理

  1. customThe aqueous layer was separated
  2. addition500 mL of CH2Cl2 was added
  3. customThe organic layer was separated
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated to dryness under vacuum

出典と根拠

ORDレコード
ord-c7dc60f6c06a446ca17c0516941f6f12
出典データセット
uspto-grants-1997_07
特許番号
US05643855

関連ノート

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