Water → N-cyclopropylpyridin-4-amine

HRID 2291510ノート

反応式

HRID 2291510 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH:15]1([NH2:18])[CH2:17][CH2:16]1.O>CN(C=O)C>[CH:15]1([NH:18][C:2]2[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=2)[CH2:17][CH2:16]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 122884-ChloropyridineHCID 69828Cyclopropylamine

生成物 1

HCID 19854218N-cyclopropylpyridin-4-amine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a magnetically stirred, 25° C. solution of 2.3 g (0.006 mol) of product of Step A and 0.71 g (0.007 mol) of triethylamine in 40 ml of DMF was added dropwise 0.38 g (0.007 mol) of cyclopropylamine. After 18 hours the reaction mixture was poured into H2O and extracted with diethyl ether. The ether phase was washed with H2O, and dried (MgSO4). The dry ether phase was concentrated in vacuo to 1.95 g of a brown solid. The crude was recrystallized from hexane/EtOAc affording 1.2 g (50%) of product as a beige solid; mp 111°-112° C.

後処理

  1. extractionextracted with diethyl ether
  2. washThe ether phase was washed with H2O
  3. dry with materialdried (MgSO4)
  4. concentrationThe dry ether phase was concentrated in vacuo to 1.95 g of a brown solid
  5. customThe crude was recrystallized from hexane/EtOAc affording 1.2 g (50%) of product as a beige solid

出典と根拠

ORDレコード
ord-2a2872fd006c4e8bb5a377e0011025ce
出典データセット
uspto-grants-1989_01
特許番号
US04797149

反応ノート

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