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Formic Acid → (1R)-2-[4-(1H-indol-4-yl)piperazin-1-yl]-2-oxo-1-(pyridin-2-ylmethyl)ethylformamide

HRID 1830607
ノート
印刷プレビュー

反応式

HRID 1830607 の反応式
[CH:1](O)=[O:2].C(OC(=O)C)(=O)C.[NH:11]1[C:19]2[C:14](=[C:15]([N:20]3[CH2:25][CH2:24][N:23]([C:26](=[O:36])[C@H:27]([NH2:35])[CH2:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=4)[CH2:22][CH2:21]3)[CH:16]=[CH:17][CH:18]=2)[CH:13]=[CH:12]1.N1(C2C=CC=C3C=2C=CN3)CCNCC1.C(OC(N[C@H](CC1C=CC=CN=1)C(O)=O)=O)(C)(C)C>C1COCC1.C(OCC)(=O)C>[NH:11]1[C:19]2[C:14](=[C:15]([N:20]3[CH2:25][CH2:24][N:23]([C:26](=[O:36])[C@H:27]([NH:35][CH:1]=[O:2])[CH2:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=4)[CH2:22][CH2:21]3)[CH:16]=[CH:17][CH:18]=2)[CH:13]=[CH:12]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

8

反応物 5

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 5945904-(piperazin-1-yl)-1H-indoleHCID 7019139(2R)-2-{[(tert-butoxy)carbonyl]amino}-3-(pyridin-2-yl)propanoic acidHCID 58651199(1R)-2-[4-(1H-indol-4-yl)piperazin-1-yl]-2-oxo-1-(pyridin-2-ylmethyl)ethylamine

生成物 1

HCID 58651198
(1R)-2-[4-(1H-indol-4-yl)piperazin-1-yl]-2-oxo-1-(pyridin-2-ylmethyl)ethylformamide

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

A mixture of formic acid (0.9 mL; 24 mmol) and acetic anhydride (1.8 mL; 19.5 mmol) was stirred at 60° C. for 4 hours, then cooled to ambient temperature. The resulting mixed anhydride was added to a −10° C. solution of (1R)-2-[4-(1H-indol-4-yl)piperazin-1-yl]-2-oxo-1-(pyridin-2-ylmethyl)ethylamine (prepared in two steps from 4-piperazin-1-yl-1H-indole and (2R)-2-[(tert-butoxycarbonyl)amino]-3-pyridin-2-ylpropanoic acid according to the procedures outlined in examples 1 and 2) (1.07 g.; 3.0 mmol) in THF (30 mL). The mixture was allowed to warm to ambient temperature over 3 hours, diluted with ethyl acetate, and washed with saturated aqueous Na2CO3. The organic layer was dried over MgSO4, filtered, and the solvent removed in vacuo. The crude residue was purified by flash chromatography to afford the title compound as a beige solid foam (720 mg.; 64%). MS EI M+.@ m/z 377; 1H NMR, 400 MHz, DMSO-d6.

後処理

  1. temperaturecooled to ambient temperature
  2. temperatureto warm to ambient temperature over 3 hours
  3. washwashed with saturated aqueous Na2CO3
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. customthe solvent removed in vacuo
  7. customThe crude residue was purified by flash chromatography

出典と根拠

ORDレコード
ord-a590c645a5b64d0c8195ee1b74806605
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07067518B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート