1,4-Dioxane → HCID 178488262、化合物

HRID 869392ノート

反応式

HRID 869392 の反応式
[Cl:1][C:2]1[C:7]2[C:8]3[NH:9][CH:10]([C:16]4[N:17]=[C:18]([CH:21]([CH3:23])[CH3:22])[S:19][CH:20]=4)[CH2:11][C:12](=[O:15])[C:13]=3[O:14][C:6]=2[CH:5]=[CH:4][C:3]=1[O:24][CH3:25].O1CCOCC1>O>[OH:15][C:12]1[CH:11]=[C:10]([C:16]2[N:17]=[C:18]([CH:21]([CH3:23])[CH3:22])[S:19][CH:20]=2)[N:9]=[C:8]2[C:7]3[C:2]([Cl:1])=[C:3]([O:24][CH3:25])[CH:4]=[CH:5][C:6]=3[O:14][C:13]=12

参加物

4

反応物 2

HCID 312751,4-DioxaneHCID 86722240HCID 86722240、化合物

生成物 1

HCID 178488262HCID 178488262、化合物収率 85.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 10B (10.3 g, 27.33 mmol, crude) and FeCl3.6H2O (33.04 g, 164.0 mmol, 6 eq) was added to 1,4-dioxane (300 mL) The mixture was refluxed for 16 hours. TLC monitored the reaction. After the reaction completed, the reaction mixture was cooled to room temperature and poured into water (300 mL), extracted with ethyl acetate and concentrated to give a crude product 10C (8.75 g), which was used for the next step directly.

後処理

  1. temperaturewas refluxed for 16 hours
  2. customthe reaction
  3. extractionextracted with ethyl acetate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-c6d8994519104d73b8fc119851e8f142
出典データセット
uspto-grants-2015_03
特許番号
US08969373B2

反応ノート

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