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Hydrochloric Acid → 4-((3,3-Dimethylcyclobutyl)(quinolin-3-ylamino)methyl)benzoic acid

HRID 2281143
ノート
印刷プレビュー

反応式

HRID 2281143 の反応式
[CH3:1][C:2]1([CH3:29])[CH2:5][CH:4]([CH:6]([NH:18][C:19]2[CH:20]=[N:21][C:22]3[C:27]([CH:28]=2)=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:7]2[CH:17]=[CH:16][C:10]([C:11]([O:13]CC)=[O:12])=[CH:9][CH:8]=2)[CH2:3]1.O1CCCC1.[OH-].[Na+].Cl>C(OCC)(=O)C.O.CO>[CH3:1][C:2]1([CH3:29])[CH2:5][CH:4]([CH:6]([NH:18][C:19]2[CH:20]=[N:21][C:22]3[C:27]([CH:28]=2)=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:7]2[CH:8]=[CH:9][C:10]([C:11]([OH:13])=[O:12])=[CH:16][CH:17]=2)[CH2:3]1
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 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 71239295Ethyl 4-((3,3-dimethylcyclobutyl)(quinolin-3-ylamino) methyl)benzoate

生成物 1

HCID 712393444-((3,3-Dimethylcyclobutyl)(quinolin-3-ylamino)methyl)benzoic acid収率 93%

試薬・触媒・溶媒 3

HCID 887
Methanol
溶媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a flask containing ethyl 4-((3,3-dimethylcyclobutyl)(quinolin-3-ylamino)methyl)benzoate (17.0 mg, 0.0440 mmol) was added tetrahydrofuran (0.110 mL), methanol (0.110 mL), and 1 N sodium hydroxide (0.110 mL, 0.110 mmol). The reaction was stirred for 18 h at room temperature. The reaction was then diluted with ethyl acetate and water. 1 N hydrochloric acid (0.110 mL) was then added dropwise to bring the pH to 3. The aqueous layer was extracted three times with ethyl acetate. The combined organic layers were dried with sodium sulfate, filtered, and concentrated to provide 4-((3,3-dimethylcyclobutyl)(quinolin-3-ylamino)methyl)benzoic acid; (14.8 mg, 93% yield) as a solid. 1H NMR (400 MHz, CDCl3) δ: 8.67 (br. s., 1H), 8.06 (d, J=8.2 Hz, 2H), 7.96 (d, J=7.4 Hz, 1H), 7.48 (d, J=8.4 Hz, 2H), 7.46-7.32 (m, 3H), 6.76 (d, J=2.5 Hz, 1H), 4.30 (d, J=9.4 Hz, 1H), 2.62-2.50 (m, 1H), 2.10-1.98 (m, 1H), 1.80-1.69 (m, 2H), 1.69-1.58 (m, 1H), 1.14 (s, 3H), 1.09 (s, 3H). MS (M+1): 361.2.

後処理

  1. extractionThe aqueous layer was extracted three times with ethyl acetate
  2. dry with materialThe combined organic layers were dried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-b3e17fb622e1481db8f878f226f0a22a
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09139538B2

反応ノート

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