Cyanamidnatrium → HCID 67053820、化合物

HRID 2171737ノート

反応式

HRID 2171737 の反応式
[N:1]#[C:2][NH2:3].[Na].[CH3:5][C:6]([O:11][C:12]1[CH:13]=[C:14]2[C:18](=[CH:19][CH:20]=1)[CH2:17][CH2:16][CH2:15]2)([C@@H:8]1[CH2:10][O:9]1)[CH3:7]>CO>[CH3:5][C:6]([O:11][C:12]1[CH:13]=[C:14]2[C:18](=[CH:19][CH:20]=1)[CH2:17][CH2:16][CH2:15]2)([CH:8]1[O:9][C:2]([NH2:3])=[N:1][CH2:10]1)[CH3:7]

参加物

4

反応物 2

HCID 57375518CyanamidnatriumHCID 86668126HCID 86668126、化合物

生成物 1

HCID 67053820HCID 67053820、化合物収率 49.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a vigorously stirred solution of sodium hydrogen cyanamide (0.21 g, 3.21 mmol) in methanol (10 mL) was added slowly (S)-2-(1,1-dimethyl-indan-5-yloxymethyl)-oxirane (0.57 g, 3.21 mmol). The reaction mixture was stirred at room temperature overnight after which the reaction mixture was concentrated. Anhydrous diethyl ether (50 mL) was added. The resulting white precipitate was filtered through Celite and the filtrate concentrated. The residue was purified by flash chromatography (silica, 7N NH3 in methanol/methylene chloride) to give 0.41 g (49%) of 5-(1,1-dimethyl-indan-5-yloxymethyl)-4,5-dihydro-oxazol-2-ylamine.

後処理

  1. concentrationwas concentrated
  2. additionAnhydrous diethyl ether (50 mL) was added
  3. filtrationThe resulting white precipitate was filtered through Celite
  4. concentrationthe filtrate concentrated
  5. customThe residue was purified by flash chromatography (silica, 7N NH3 in methanol/methylene chloride)

出典と根拠

ORDレコード
ord-6925a7995f484976921716c35a678614
出典データセット
uspto-grants-2015_06
特許番号
US09051331B2

反応ノート

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