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1-Naphthoic acid → HCID 178478885、化合物

HRID 394551
ノート
印刷プレビュー

反応式

HRID 394551 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][C:13]1[N:14]=[CH:15][NH:16][CH:17]=1)[CH2:7][CH:6]([NH2:18])[CH2:5]2.ON1C2C=CC=NC=2N=N1.[C:29]1([C:39](O)=[O:40])[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[CH:32]=[CH:31][CH:30]=1.C(N(C(C)C)CC)(C)C.[ClH:51].CN(C)CCCN=C=NCC>CN(C)C=O.C(Cl)(Cl)Cl>[ClH:51].[ClH:51].[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][C:13]1[N:14]=[CH:15][NH:16][CH:17]=1)[CH2:7][CH:6]([NH:18][C:39]([C:29]1[C:38]3[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=3)[CH:32]=[CH:31][CH:30]=1)=[O:40])[CH2:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 68471-Naphthoic acidHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 116798243H-1,2,3-Triazolo[4,5-b]pyridine, 1-oxideHCID 178507189HCID 178507189、化合物

生成物 1

HCID 178478885HCID 178478885、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 6-Bromo-1,2,3,4-tetrahydro-1-(1H-imidazol-4-ylmethyl)-3-quinolinamine (30 mg, 0.072 mmol) in dimethyl formamide (1 mL) were sequentially added 1-hydroxyazabenzotriazole (19 mg, 0.15 mmol), 1-naphthoic acid (25 mg, 0.15 mmol), diisopropylethyl amine (0.7 mL, 0.4 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (28 mg, 0.15 mmol). After 18 hours, the mixture was diluted with chloroform (10 mL) and washed with saturated NaHCO3 solution (10 mL). The organic layer was separated, dried and concentrated. Purification by silica gel flash column chromatography eluting with 50% ethyl acetate in hexanes followed by 1:9 methanol in chloroform afforded two fractions. More polar fraction 2 (14 mg) was the desired product and the less polar fraction 1 (35 mg) was diacylated product. Fraction 1 was dissolved in methanol (1 mL) and treated with NaOH solution (1 N, 0.2 mL). After 30 minutes, the mixture was concentrated and mixed with fraction 2 obtained above. The resulting mixture was dissolved in chloroform (10 mL) and washed with water (10 mL). The organic layer was dried (MgSO4), concentrated and purified by silica gel flash column eluting with 5% methanol in chloroform to afford the free base of the title compound (20 mg, 60%). The solid was dissolved in chloroform and HCl gas was bubbled for 30 seconds. The mixture was then concentrated in vacuo to afford the title compund (23 mg). MS: (M+H)+=461, 463 (1:1 ratio), 1 Br pattern.

後処理

  1. washwashed with saturated NaHCO3 solution (10 mL)
  2. customThe organic layer was separated
  3. customdried
  4. concentrationconcentrated
  5. customPurification by silica gel flash column chromatography
  6. washeluting with 50% ethyl acetate in hexanes
  7. customafforded two fractions

出典と根拠

ORDレコード
ord-6005e7bc81c2424aa607465cab94f1b0
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06602883B1

反応ノート

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