Triethylamine → HCID 57687386、化合物

HRID 559064

反応式

HRID 559064 の反応式
[F:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7](F)[C:3]=1[C:4]([OH:6])=[O:5].Cl.CN.[CH2:16]([N:18](CC)CC)C>N1C=CC=CC=1>[F:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]([NH:18][CH3:16])[C:3]=1[C:4]([OH:6])=[O:5]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 5203732,4,6-Trifluorobenzoic acidHCID 6364545Methylamine hydrochloride

生成物 1

HCID 57687386HCID 57687386、化合物収率 91.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
110 °C

実験手順

To a solution of 2,4,6-trifluorobenzoic acid (6.0 g, 34.1 mmol) and methylamine hydrochloride (12.0 g, 170 mmol) in pyridine (24 mL), triethylamine (24 mL, 170 mmol) was added. The reaction was stirred at 110° C. for 15 h and then concentrated in vacuo. The residue was acidified with 1N HCl (100 mL). The precipitate was collected by filtration to give 5.83 g of clean desired product as an orange solid (91%). 1H NMR (400 MHz, DMS O-d6): δ 13.09 (s, 1H), 7.91 (s, 1H), 6.33 (s, 1H), 6.30 (s, 1H), 2.81 (s, 3H). MS (ES) [m+H] calc'd for C8H7F2NO2, 188; found 188.

後処理

  1. concentrationconcentrated in vacuo
  2. filtrationThe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-62369ebfb3254567a049c2f849592993
出典データセット
uspto-grants-2011_11
特許番号
US08063066B2

関連ノート

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