HCID 86617954, 화합물 → HCID 57798317, 화합물

HRID 2100316노트

반응식

HRID 2100316 반응식
C1(C(C2C=CC=CC=2)[N:8]2[CH2:11][C:10]([CH2:18][NH:19][C:20](=[O:26])[O:21][C:22]([CH3:25])([CH3:24])[CH3:23])([N:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)[CH2:9]2)C=CC=CC=1>CO.[OH-].[OH-].[Pd+2]>[N:12]1([C:10]2([CH2:18][NH:19][C:20](=[O:26])[O:21][C:22]([CH3:24])([CH3:23])[CH3:25])[CH2:11][NH:8][CH2:9]2)[CH2:13][CH2:14][O:15][CH2:16][CH2:17]1

참가 물질

4

반응물 1

HCID 86617954HCID 86617954, 화합물

생성물 1

HCID 57798317HCID 57798317, 화합물

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 887Methanol용매

실험 절차

[1-(diphenylmethyl)-3-morpholin-4-ylazetidin-3-yl]methyl}amine (1.00 g, 3.0 mmol) was dissolved in dichloromethane (10 ml) and di-tert-butyldicarbonate (0.71 g, 3.3 mmol) was added. This was followed by the dropwise addition of triethylamine (0.62 ml, 4.4 mmol). The reaction was stirred at room temperature overnight. The organics were washed with water, dried over anhydrous magnesium sulfate and evaporated to dryness to give tert-butyl {[1-(diphenylmethyl)-3-morpholin-4-ylazetidin-3-yl]methyl}carbamate. tert-butyl {[1-(diphenylmethyl)-3-morpholin-4-ylazetidin-3-yl]methyl}carbamate (1.20 g, 2.7 mmol) and 20% palladium hydroxide on carbon (0.12 g) in methanol (20 ml) was hydrogenated on a parr at 45 psi for 2 days (complete conversion to product by 1c-ms). The resulting mixture was filtered and the filtercake washed with methanol. The methanol was evaporated to give tert-butyl [(3-morpholin-4-ylazetidin-3-yl)methyl]carbamate which was used without further purification. m/z (M++H) 272.

후처리

  1. filtrationThe resulting mixture was filtered
  2. washthe filtercake washed with methanol
  3. customThe methanol was evaporated

출처 및 근거

ORD 기록
ord-076c7464529745409cf1f5c67c86f380
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07572792B2

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