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Sodium Bicarbonate → HCID 59626746、化合物

HRID 2400374
ノート
印刷プレビュー

反応式

HRID 2400374 の反応式
[CH2:1]([O:8][C:9]([NH:11][CH:12]([CH2:17][C:18]1[C:19]([CH2:28][NH:29][CH2:30][C:31]2[CH:36]=[CH:35][C:34]([O:37][CH3:38])=[CH:33][CH:32]=2)=[C:20]2[C:24](=[C:25]([Cl:27])[CH:26]=1)[NH:23][N:22]=[CH:21]2)[C:13]([O:15]C)=O)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1>[Cl:27][C:25]1[C:24]2[NH:23][N:22]=[CH:21][C:20]=2[C:19]2[CH2:28][N:29]([CH2:30][C:31]3[CH:32]=[CH:33][C:34]([O:37][CH3:38])=[CH:35][CH:36]=3)[C:13](=[O:15])[CH:12]([NH:11][C:9](=[O:10])[O:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH2:17][C:18]=2[CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 59626688HCID 59626688、化合物

生成物 1

HCID 59626746HCID 59626746、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of Methyl 2-{[(benzyloxy)carbonyl]amino}-3-(7-chloro-4-{[(4-methoxybenzyl)amino]methyl}-1H-indazol-5-yl)propanoate from Step A in toluene (100 mL) was heated at reflux for 3 hours and then cooled to room temperature. The reaction mix was poured into a saturated aqueous solution of sodium bicarbonate and the mixture was extracted with Ethyl acetate (2×200 mL). The combined organic extracts were washed once with brine (100 mL), dried over anhydrous sodium sulfate, filtered and concentrated at reduced pressure. The resulting solid was swished once with a 1:1 mix of ethylacetate/hexane and the solid collected by filtration to give 3.1 g of the title compound to give the title compound. MS: m/z 505 (M+1).

後処理

  1. temperatureat reflux for 3 hours
  2. additionThe reaction mix
  3. extractionthe mixture was extracted with Ethyl acetate (2×200 mL)
  4. washThe combined organic extracts were washed once with brine (100 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated at reduced pressure
  8. additionmix of ethylacetate/hexane
  9. filtrationthe solid collected by filtration

出典と根拠

ORDレコード
ord-083a2625ae25469b8deaf73d6da73376
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08796260B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート