Ethanol → HCID 21196274、化合物

HRID 1108248ノート

反応式

HRID 1108248 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 title 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-5905590d114344df82c850215802f094
出典データセット
uspto-grants-2000_05
特許番号
US06066638

反応ノート

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