Cysteamine Hydrochloride → HCID 20213304、化合物

HRID 65740ノート

反応式

HRID 65740 の反応式
Cl.[NH2:2][CH2:3][CH2:4][SH:5].CC(C)([O-])C.[K+].C(O[CH2:16][C:17]1[O:18][C:19]([CH2:22][CH2:23][CH2:24][CH2:25][N:26]([CH3:28])[CH3:27])=[CH:20][CH:21]=1)(=O)C>CN(C)C=O.CO>[CH3:28][N:26]([CH3:27])[CH2:25][CH2:24][CH2:23][CH2:22][C:19]1[O:18][C:17]([CH2:16][S:5][CH2:4][CH2:3][NH2:2])=[CH:21][CH:20]=1

参加物

6

反応物 3

HCID 9082Cysteamine HydrochlorideHCID 23452115[5-[4-(Dimethylamino)butyl]-2-furanyl]methyl ethanoateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 20213304HCID 20213304、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

Cysteamine hydrochloride (4.5 g) was added to a cooled solution of potassium-t-butoxide (8.98 g) in dry dimethylformamide (125 ml). The mixture was stirred for 20 min and [5-[4-(dimethylamino)butyl]-2-furanyl]methyl ethanoate (9.6 g) was added. The reaction was heated at 90° for 4 hr, poured onto an ice-water mixture and extracted with chloroform. Distillation of the organic extract gave a yellow oil which after column chromatography on silica, using methanol/0.880 ammonia (9:1) as eluent, and a further distillation afforded a colourless oil b.p. 140°/0.05 mm Hg. Found: C, 60.81; H, 9.86; N, 10.44. Calc. for C13H24N2OS: C, 60.91; H, 9.44; N, 10.93%.

後処理

  1. temperatureThe reaction was heated at 90° for 4 hr
  2. extractionextracted with chloroform
  3. distillationDistillation of the
  4. extractionorganic extract
  5. customgave a yellow oil which after column chromatography on silica
  6. distillationa further distillation

出典と根拠

ORDレコード
ord-3fbcb9616b764f8b86c0f958fa12c163
出典データセット
uspto-grants-1978_12
特許番号
US04128658

反応ノート

読み込み中…