HCID 86617954、化合物 → HCID 57798317、化合物

HRID 2100316ノート

反応式

HRID 2100316 の反応式
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

参加物

4

反応物 1

HCID 86617954HCID 86617954、化合物

生成物 1

HCID 57798317HCID 57798317、化合物

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 887Methanol溶媒

実験手順

[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.

後処理

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

出典と根拠

ORDレコード
ord-076c7464529745409cf1f5c67c86f380
出典データセット
uspto-grants-2009_08
特許番号
US07572792B2

反応ノート

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