HCID 68552376、化合物 → 460078-00-6
反応式
COC1C=CC(C[NH:8][CH2:9][CH2:10][CH:11]([CH2:24][CH2:25][NH:26]CC2C=CC(OC)=CC=2)[CH2:12][CH2:13][NH:14]CC2C=CC(OC)=CC=2)=CC=1>CO.[OH-].[OH-].[Pd+2]>[NH2:8][CH2:9][CH2:10][CH:11]([CH2:24][CH2:25][NH2:26])[CH2:12][CH2:13][NH2:14]参加物
4
実験手順
1,1,1-tris[2-(p-methoxybenzylamino)ethyl]methane (20.0 gram, 0.036 mol) was dissolved in methanol (100 ml) and Pd(OH)2 (5.0 gram) was added. The mixture was hydrogenated (3 bar, 100° C., in an autoclave) and stirred for 5 hours. Pd(OH)2 was added in two more portions (2×5 gram) after 10 and 15 hours respectively. The reaction mixture was filtered and the filtrate was washed with methanol. The combined organic phase was evaporated and the residue was distilled under vacuum (1×10−2, 110° C.) to give 2.60 gram (50%) of 1,1,1-tris(2-aminoethyl)methane.
後処理
- custom3 bar, 100° C.
- filtrationThe reaction mixture was filtered
- washthe filtrate was washed with methanol
- customThe combined organic phase was evaporated
- distillationthe residue was distilled under vacuum (1×10−2, 110° C.)
出典と根拠
- ORDレコード
- ord-d206a18aa2c64e3da3dc01feae369ba2
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08304388B2
反応ノート
読み込み中…