Cyanamidnatrium → HCID 67053820, 화합물

HRID 2171737노트

반응식

HRID 2171737 반응식
[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]

참가 물질

4

반응물 2

HCID 57375518CyanamidnatriumHCID 86668126HCID 86668126, 화합물

생성물 1

HCID 67053820HCID 67053820, 화합물수율 49.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-6925a7995f484976921716c35a678614
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051331B2

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