Triethylamine → HCID 53885292、化合物

HRID 1637115ノート

反応式

HRID 1637115 の反応式
Cl.[NH2:2][CH2:3][CH:4]([C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([O:21][CH:22]2[CH2:26][CH2:25][CH2:24][CH2:23]2)[CH:14]=1)[C:5]#[C:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.CCN(CC)CC.[F:34][C:35]([F:42])([F:41])[C:36](OCC)=[O:37]>CO>[CH:22]1([O:21][C:15]2[CH:14]=[C:13]([CH:4]([C:5]#[C:6][C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=3)[CH2:3][NH:2][C:36](=[O:37])[C:35]([F:42])([F:41])[F:34])[CH:18]=[CH:17][C:16]=2[O:19][CH3:20])[CH2:26][CH2:25][CH2:24][CH2:23]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 9794Ethyl trifluoroacetateHCID 573652252-[3-(Cyclopentyloxy)-4-methoxyphenyl]-4-phenylbut-3-yn-1-amine--hydrogen chloride (1/1)

生成物 1

HCID 53885292HCID 53885292、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of (+/-)-4-amino-3-(3-cyclopentyloxy-4-methoxyphenyl)-1-phenyl-1-butyne hydrochloride (50 mg, 0.14 mmol) and Et3N (40 mg) in a mixture of MeOH (1 ml) and ethyl trifluoroacetate (0.5 ml) was refluxed overnight. The solvents were evaporated, the residue taken up in Et2O, washed with H2O, 0.01N HCl, dried, and the solvent evaporated. The residue was crystallized from a mixture of cyclohexane and Et2O, and gave the titled compound, 32 mg (55%). mp 143-145°. 1H NMR (400 MHz, CDCl3) δ 7.42 (m, 2 H), 7.32 (m, 3 H), 6.94 (m, 2 H), 6.84 (d, 1 H), 6.54 (broad s, 1 H), 4.78 (m, 1 H), 4.08 (t, 1 H), 3.82 (s, 3 H), 3.78 (m, 1 H), 3.58 (m, 1 H), 1.76-1.92 (m, 6 H), 1.60 (m, 2 H).

後処理

  1. temperaturewas refluxed overnight
  2. customThe solvents were evaporated
  3. washwashed with H2O, 0.01N HCl
  4. customdried
  5. customthe solvent evaporated
  6. customThe residue was crystallized from a mixture of cyclohexane and Et2O

出典と根拠

ORDレコード
ord-eddb1cbff0b84f55b4dc47b529f5106e
出典データセット
uspto-grants-2000_03
特許番号
US06037367

反応ノート

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