Triethylamine → Methyl 6-[(2,3-dihydroxypropyl)amino]-3-nitropyrazine-2-carboxylate

HRID 64612

反応式

HRID 64612 の反応式
Cl[C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[C:5]([N+:12]([O-:14])=[O:13])=[N:4][CH:3]=1.[NH2:15][CH2:16][CH:17]([OH:20])[CH2:18][OH:19].C(N(CC)CC)C>C(O)(C)C>[OH:20][CH:17]([CH2:18][OH:19])[CH2:16][NH:15][C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[C:5]([N+:12]([O-:14])=[O:13])=[N:4][CH:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 735613-Amino-1,2-propanediolHCID 15914238Methyl 6-chloro-3-nitropyrazine-2-carboxylate

生成物 1

HCID 15914243Methyl 6-[(2,3-dihydroxypropyl)amino]-3-nitropyrazine-2-carboxylate

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

To 1.0 g (0.004 mol) 9 in 15 ml isopropanol is added 0.36 g (0.004 mol) 10 and 0.4 g (0.004 mol) triethylamine at room temperature. The reaction mixture becomes reddish in color and is stirred at room temperature for 16 hours. The solvent is removed on the rotary evaporator and the residue is purified by flash chromatography on silica gel followed by elution with 10% methanol/chloroform. Pure 15 has Rf 0.4 and is obtained as a yellow solid, m.p. 107°-9°.

後処理

  1. customThe solvent is removed on the rotary evaporator
  2. customthe residue is purified by flash chromatography on silica gel
  3. washfollowed by elution with 10% methanol/chloroform
  4. customis obtained as a yellow solid, m.p. 107°-9°

出典と根拠

ORDレコード
ord-454a61fe3d5d40748003eece1dae88cf
出典データセット
uspto-grants-1986_09
特許番号
US04609659

関連ノート

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