Triethylamine → HCID 53885292, 화합물

HRID 1637115노트

반응식

HRID 1637115 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 53885292HCID 53885292, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-eddb1cbff0b84f55b4dc47b529f5106e
출처 데이터셋
uspto-grants-2000_03
특허 번호
US06037367

반응 노트

불러오는 중…