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Lithium Hydroxide → (S)-N-({6-[(3-methyl-1-{4-[5-(trifluoromethyl)pyridin-2-yl]phenyl}butyl)amino]pyridin-3-yl}carbonyl)-beta-alanine

HRID 2173833
ノート
印刷プレビュー

反応式

HRID 2173833 の反応式
[CH3:1][CH:2]([CH3:38])[CH2:3][C@H:4]([NH:21][C:22]1[N:27]=[CH:26][C:25]([C:28]([NH:30][CH2:31][CH2:32][C:33]([O:35]CC)=[O:34])=[O:29])=[CH:24][CH:23]=1)[C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][N:12]=2)=[CH:7][CH:6]=1.O1CCCC1.[OH-].[Li+]>CO>[CH3:1][CH:2]([CH3:38])[CH2:3][C@H:4]([NH:21][C:22]1[N:27]=[CH:26][C:25]([C:28]([NH:30][CH2:31][CH2:32][C:33]([OH:35])=[O:34])=[O:29])=[CH:24][CH:23]=1)[C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][N:12]=2)=[CH:7][CH:6]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 68061979(S)-ethyl N-({6-[(3-methyl-1-{4-[5-(trifluoromethyl)pyridin-2-yl]phenyl}butyl)amino]pyridin-3-yl}carbonyl)-beta-alaninate

生成物 1

HCID 67981277(S)-N-({6-[(3-methyl-1-{4-[5-(trifluoromethyl)pyridin-2-yl]phenyl}butyl)amino]pyridin-3-yl}carbonyl)-beta-alanine収率 87%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

反応条件

温度
50 °C

実験手順

A mixture of (S)-ethyl N-({6-[(3-methyl-1-{4-[5-(trifluoromethyl)pyridin-2-yl]phenyl}butyl)amino]pyridin-3-yl}carbonyl)-beta-alaninate (60.9 g, 115 mmol) was dissolved in methanol (230 ml) and tetrahydrofuran (115 ml) and treated with aqueous lithium hydroxide (115 ml, 0.230 mol, 2.0M). The reaction was heated to 50° C. for 30 minutes. The solution was concentrated in vacuo, and the resulting residue was diluted with water (approximately 500 ml). The mixture was then acidified with aqueous 1.0M hydrochloric acid (230 ml, to approximately pH 4.0). The precipitated solid was collected by filtration and washed with water (2×100 ml). Air was pulled through the filter cake over 12 hours to affect drying of the product. The crude solid was transferred into a 2-liter flask with a stirbar and the solid was suspended in ethyl acetate (approximately 1.5 L). Sodium sulfate (approximately 500 g) was added and the mixture was stirred vigorously for a further 1 hour. The cloudy mixture was filtered through a plug of celite, resulting in a clear solution. The solution was concentrated in vacuo and the remaining solid was suspended in diethyl ether (1 L) and concentrated in vacuo (the process was repeated twice). The resulting solid was pulverized with a mortar and pestel, and dried in a vacuum oven for 12 hours at 60° C. The final product (50.1 g, 87%) was obtained as a off-white solid. 1H NMR (400 MHz, DMSO-d6, δ): 9.01 (s, 1H), 8.39 (d, J=1.2 Hz, 1H), 8.26 (dd, J=8.4, 2.0 Hz, 2H), 8.15 (d, J=8.4 Hz, 1H), 8.10 (d, J=8.2 Hz, 2H), 7.84 (d, J=6.7 Hz, 1H), 7.55 (d, J=8.2 Hz, 2H), 6.66 (br. s., 1H), 5.15 (br. s., 1H), 3.33-3.43 (m, 2H), 2.45 (t, J=7.0 Hz, 2H), 1.74-1.86 (m, 1H), 1.62-1.72 (m, 1H), 1.51-1.62 (m, 1H), 0.95 (d, J=6.5 Hz, 3H), 0.92 (d, J=6.5 Hz, 3H). MS (M+1): 501.4.

後処理

  1. concentrationThe solution was concentrated in vacuo
  2. additionthe resulting residue was diluted with water (approximately 500 ml)
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water (2×100 ml)
  5. customto affect drying of the product
  6. customThe crude solid was transferred into a 2-liter flask with a stirbar
  7. additionSodium sulfate (approximately 500 g) was added
  8. filtrationThe cloudy mixture was filtered through a plug of celite
  9. customresulting in a clear solution
  10. concentrationThe solution was concentrated in vacuo
  11. concentrationconcentrated in vacuo (the process
  12. customdried in a vacuum oven for 12 hours at 60° C

出典と根拠

ORDレコード
ord-984338df28344b65bc13da0e3bdf8fec
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09056834B2

反応ノート

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