Tris(hydroxymethyl)aminomethane → Methyl {4-[({[(4-tert-butylphenyl)amino]carbonyl}{4-[(4-butylphenyl)-ethynyl]benzyl}amino)methyl]phenoxy}acetate

HRID 551897

反応式

HRID 551897 の反応式
[CH2:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]#[C:12][C:13]2[CH:33]=[CH:32][C:16]([CH2:17][NH:18][CH2:19][C:20]3[CH:31]=[CH:30][C:23]([O:24][CH2:25][C:26]([O:28][CH3:29])=[O:27])=[CH:22][CH:21]=3)=[CH:15][CH:14]=2)=[CH:7][CH:6]=1)[CH2:2][CH2:3][CH3:4].[C:34]([C:38]1[CH:43]=[CH:42][C:41]([N:44]=[C:45]=[O:46])=[CH:40][CH:39]=1)([CH3:37])([CH3:36])[CH3:35].N1CCOCC1.C(O)C(N)(CO)CO>C(Cl)Cl>[C:34]([C:38]1[CH:43]=[CH:42][C:41]([NH:44][C:45]([N:18]([CH2:19][C:20]2[CH:21]=[CH:22][C:23]([O:24][CH2:25][C:26]([O:28][CH3:29])=[O:27])=[CH:30][CH:31]=2)[CH2:17][C:16]2[CH:15]=[CH:14][C:13]([C:12]#[C:11][C:8]3[CH:7]=[CH:6][C:5]([CH2:1][CH2:2][CH2:3][CH3:4])=[CH:10][CH:9]=3)=[CH:33][CH:32]=2)=[O:46])=[CH:40][CH:39]=1)([CH3:37])([CH3:35])[CH3:36]

参加物

6

反応物 4

HCID 6503Tris(hydroxymethyl)aminomethaneHCID 8083MorpholineHCID 27356951-Tert-butyl-4-isocyanatobenzeneHCID 57554567Methyl {4-[({4-[(4-butylphenyl)ethynyl]benzyl}amino)methyl]phenoxy}acetate

生成物 1

HCID 11541808Methyl {4-[({[(4-tert-butylphenyl)amino]carbonyl}{4-[(4-butylphenyl)-ethynyl]benzyl}amino)methyl]phenoxy}acetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of methyl {4-[({4-[(4-butylphenyl)ethynyl]benzyl}amino)methyl]phenoxy}acetate (45 mg, 0.10 mmol) and 4-tert-butylphenylisocyanate (Aldrich, 27 mg, 0.15 mmol) in DCM (2 mL) was stirred at rt overnight in presence of a morpholine resin (1.5 eq., Novabiochem HL, 3.8 mmol/g). Trisamine resin (1.2 eq, Novabiochem, 3.5 mmol/g) was then added and the mixture was stirred at rt for an additional 2 hrs. The reaction mixture was then filtrated and the solvent was removed under reduced pressure to give quantitatively the title compound. HPLC, Rt: 5.97 min purity: 96.3%). M+(ESI): 619.6, M−(ESI): 616.9.

後処理

  1. filtrationThe reaction mixture was then filtrated
  2. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-e3844b273548408292ebf116bfd0dabc
出典データセット
uspto-grants-2011_05
特許番号
US07947851B2

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