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Hydrochloric Acid → HCID 178420090、化合物

HRID 2407682
ノート
印刷プレビュー

反応式

HRID 2407682 の反応式
[C:1]1([C:7]2[CH:11]=[C:10]([CH2:12][N:13]3[CH2:18][CH2:17][CH:16]([CH2:19][NH:20][C:21]4[C:29]5[C:24](=[CH:25][CH:26]=[C:27]([C:30]6[N:34]=[CH:33][N:32](C(C7C=CC=CC=7)(C7C=CC=CC=7)C7C=CC=CC=7)[N:31]=6)[CH:28]=5)[N:23](C5CCCCO5)[N:22]=4)[CH2:15][CH2:14]3)[O:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.Cl.C(=O)(O)[O-].[Na+]>O1CCCC1.O>[C:1]1([C:7]2[CH:11]=[C:10]([CH2:12][N:13]3[CH2:14][CH2:15][CH:16]([CH2:19][NH:20][C:21]4[C:29]5[C:24](=[CH:25][CH:26]=[C:27]([C:30]6[N:34]=[CH:33][NH:32][N:31]=6)[CH:28]=5)[NH:23][N:22]=4)[CH2:17][CH2:18]3)[O:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 516892Sodium BicarbonateHCID 58504049HCID 58504049、化合物

生成物 1

HCID 178420090HCID 178420090、化合物収率 52.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

The compound prepared in Example 72 (0.13 g) was suspended in a mixture of tetrahydrofuran (6 mL), methanol (6 mL), water (1.5 mL) and concentrated hydrochloric acid (1.5 mL) and heated at reflux overnight. The reaction mixture was cooled to room temperature and poured into a saturated aqueous sodium bicarbonate solution and extracted into ethyl acetate. The organics were dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel to obtain the title compound (0.040 g) having the following physical data.

後処理

  1. temperatureheated
  2. temperatureat reflux overnight
  3. extractionextracted into ethyl acetate
  4. dry with materialThe organics were dried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-420e3f148f8c4f4c9522f5bb1dfbd503
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809538B2

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