Tetrahydrofuran → HCID 86664952、化合物

HRID 74291ノート

反応式

HRID 74291 の反応式
Cl.[NH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][C:12]([C:14]3[O:15][C:16]4[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=4[N:18]=3)=[CH:13][C:8]=2[N:7]=[C:6]1[CH3:23].[CH3:24][N:25]=[C:26]=[S:27].C(N(CC)CC)C.C1COCC1>O.C(Cl)(Cl)Cl>[O:15]1[C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[N:18]=[C:14]1[C:12]1[CH:11]=[CH:10][C:9]2[N:5]([CH2:4][CH2:3][NH:2][C:26](=[S:27])[NH:25][CH3:24])[C:6]([CH3:23])=[N:7][C:8]=2[CH:13]=1

参加物

7

反応物 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 11167Methyl isothiocyanateHCID 674977031-(2-Aminoethyl)-5-(benzoxazol-2-yl)-2-methylbenzimidazole hydrochloride

生成物 1

HCID 86664952HCID 86664952、化合物収率 40%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

1-(2-Aminoethyl)-5-(benzoxazol-2-yl)-2-methylbenzimidazole hydrochloride (see Working Example 56) (0.20 g, 0.6 mmol), methyl isothiocyanate (0.17 g, 0.6 mmol), triethylamine (0.13 g, 13 mmol) and THF (2 mL) were added together, and stirred for 1 hour at room temperature. After cooling, chloroform and water were added and extraction was carried out. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. The solid obtained was separated by filtration and dried to yield the title compound (0.08 g, 40% yield) as white crystals.

後処理

  1. temperatureAfter cooling
  2. extractionextraction
  3. customAfter the organic layer obtained
  4. dry with materialwas dried over anhydrous sodium sulfate, it
  5. filtrationwas filtered
  6. concentrationconcentrated
  7. customThe solid obtained
  8. customwas separated by filtration
  9. customdried

出典と根拠

ORDレコード
ord-2a8d93b5a41341c3a3b0bf5871e0ab9f
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

反応ノート

読み込み中…