Ethanolamine → HCID 86622763、化合物

HRID 1020264ノート

反応式

HRID 1020264 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][C:19]=1[Cl:20])[CH2:5][NH:6][C:7]([NH:9][C:10]1[S:11][CH:12]=[C:13]([CH2:15]I)[N:14]=1)=[O:8].[NH2:21][CH2:22][CH2:23][OH:24].O>C1COCC1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][C:19]=1[Cl:20])[CH2:5][NH:6][C:7]([NH:9][C:10]1[S:11][CH:12]=[C:13]([CH2:15][NH:21][CH2:22][CH2:23][OH:24])[N:14]=1)=[O:8]

参加物

5

反応物 3

HCID 700EthanolamineHCID 962WaterHCID 58055059HCID 58055059、化合物2 回

生成物 1

HCID 86622763HCID 86622763、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1-(3,4-dichlorobenzyl)-3-(4-(iodomethyl)thiazol-2-yl)urea (Intermediate XXII) was taken up in THF and an excess of the 2-Amino-ethanol (20 equiv.) was added. The reaction was allowed to stir overnight at room temperature. Reaction poured into water and extracted with ethyl acetate, partitioned with brine, dried over NaSO4, filtered, and volatiles were removed in vacuo. The resulting solid was triturated with ethyl acetate, followed by diethyl ether to give the title compound. 1H NMR (400 MHz, CD3OD): 7.50-7.45 (m, 2H), 7.26 (dd, 1H), 6.78 (s, 1H), 4.41 (s, 2H), 3.73 (s, 2H), 3.65 (t, 2H), 2.71 (t, 2H). MS (ES+): M/Z 375 and 377 (M+1).

後処理

  1. customReaction
  2. extractionextracted with ethyl acetate
  3. custompartitioned with brine
  4. dry with materialdried over NaSO4
  5. filtrationfiltered
  6. customvolatiles were removed in vacuo
  7. customThe resulting solid was triturated with ethyl acetate

出典と根拠

ORDレコード
ord-0bcf118631424f68ac5b317637b6f4e4
出典データセット
uspto-grants-2014_05
特許番号
US08716320B2

反応ノート

読み込み中…