Ethanol → HCID 21196274、化合物

HRID 1066874ノート

反応式

HRID 1066874 の反応式
[CH2:1]([N:4]=[C:5]=[S:6])[CH2:2][CH3:3].C(N(CC)CC)C.Br.[NH2:15][C:16]1[C:21]([C:22]([OH:24])=O)=[CH:20][C:19]([Br:25])=[CH:18][N:17]=1.C(O)C>CN(C)C=O>[Br:25][C:19]1[CH:18]=[N:17][C:16]2[NH:15][C:5](=[S:6])[N:4]([CH2:1][CH2:2][CH3:3])[C:22](=[O:24])[C:21]=2[CH:20]=1

参加物

6

反応物 4

HCID 702EthanolHCID 8471TriethylamineHCID 69403Propyl IsothiocyanateHCID 573505542-Amino-5-bromopyridine-3-carboxylic acid--hydrogen bromide (1/1)

生成物 1

HCID 21196274HCID 21196274、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of n-propyl isothiocyanate (1.59 g, 1.62 mL), triethylamine (5.0 g, 13.8 mL), and 5.0 g of the tide compound of Step A was heated to 100-110° C. in 22 mL of dimethylformamide for 48 h. The reaction mixture was then allowed to cool to room temperature and treated with 10 mL of ethanol. The resulting precipitate was filtered, washed with ethanol followed by hexanes and dried to deliver 2.48 g of the title compound of Step B. 1H NMR (400 MHz, Me2SO-d6): δ 0.90 (t,3H), 1.60-1.78 (m,2H), 4.30 (t,2H), 8.41 (s,1H), 8.82 (s,1H), 13.55 (s,1H).

後処理

  1. filtrationThe resulting precipitate was filtered
  2. washwashed with ethanol
  3. customdried

出典と根拠

ORDレコード
ord-09b4c2d49279414ca0e928787f4c4d06
出典データセット
uspto-grants-2001_06
特許番号
US06245770B1

反応ノート

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