Tert-Butylamine → HCID 66661120、化合物

HRID 408873

反応式

HRID 408873 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]([OH:10])=O)[CH:3]=1.C(N(CC)CC)C.[C:18]([NH2:22])([CH3:21])([CH3:20])[CH3:19].CCCP1(OP(CCC)(=O)OP(CCC)(=O)O1)=O>ClCCl>[C:18]([NH:22][C:8](=[O:10])[C:4]1[CH:3]=[C:2]([CH3:1])[CH:7]=[CH:6][N:5]=1)([CH3:21])([CH3:20])[CH3:19]

参加物

6

反応物 4

HCID 6385Tert-ButylamineHCID 8471TriethylamineHCID 111923Propylphosphonic anhydrideHCID 27628204-Methylpyridine-2-carboxylic acid

生成物 1

HCID 66661120HCID 66661120、化合物収率 53.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-Methylpyridine-2-carboxylic acid (500 mg, 3.65 mmol), triethylamine (1.27 g, 12.5 mmol, 1.75 mL) and tert-butylamine (267 mg, 3.65 mmol) were combined and stirred in dichloromethane (1 mL). 1-Propanephosphonic acid cyclic anhydride (4.82 g, 7.5 mmol, 4.5 mL, 50% solution in ethyl acetate) was added dropwise and the reaction stirred at room temperature for 1 hour. The reaction mixture was concentrated at reduced pressure and the resulting residue taken up in ethyl acetate and washed with saturated sodium bicarbonate solution. The organic phase was dried over sodium sulfate and concentrated under vacuum to afford the title compound (376 mg). MS (ESI) m/z 193.4 [M+H]+

後処理

  1. concentrationThe reaction mixture was concentrated at reduced pressure
  2. washwashed with saturated sodium bicarbonate solution
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-56b48c9a327b4901b2f453bf902d264d
出典データセット
uspto-grants-2014_06
特許番号
US08759352B2

関連ノート

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