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Potassium Iodide → 1,1'-(9H-Thioxanthene-2,7-diyl)bis[4-(diethylamino)butan-1-one]--hydrogen chloride (1/2)

HRID 1076894
ノート
印刷プレビュー

反応式

HRID 1076894 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:20]=[CH:19][C:18]2[S:17][C:16]3[C:11](=[CH:12][C:13]([C:21](=[O:26])[CH2:22][CH2:23][CH2:24]Cl)=[CH:14][CH:15]=3)[CH2:10][C:9]=2[CH:8]=1)=[O:6].[I-].[K+].[CH2:29]([NH:31][CH2:32][CH3:33])[CH3:30]>O1CCCC1>[ClH:1].[ClH:1].[CH2:29]([N:31]([CH2:32][CH3:33])[CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:20]=[CH:19][C:18]2[S:17][C:16]3[C:11](=[CH:12][C:13]([C:21](=[O:26])[CH2:22][CH2:23][CH2:24][N:31]([CH2:32][CH3:33])[CH2:29][CH3:30])=[CH:14][CH:15]=3)[CH2:10][C:9]=2[CH:8]=1)=[O:6])[CH3:30]
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 4875Potassium IodideHCID 8021DiethylamineHCID 12340288HCID 12340288、化合物

生成物 1

HCID 123402921,1'-(9H-Thioxanthene-2,7-diyl)bis[4-(diethylamino)butan-1-one]--hydrogen chloride (1/2)

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
110 °C

実験手順

A mixture of 32.6 g (0.08 mole) of 2,7-bis(4-chlorobutyryl)thioxanthene, 2 g of potassium iodide, 100 ml of diethylamine and 100 ml of tetrahydrofuran was heated for 24 hours with stirring in a Paar bomb at 110°C. Upon cooling the mixture was evaporated to near dryness. The residue was dissolved in methylene chloride, washed with water then with saturated NaCl solution, dried over magnesium sulfate and filtered. The filtrate was evaporated to near dryness and recrystallized several times from methanol-diethyl ether and from acetone-methanol to give the desired product. M.P. 188°-191°C.

後処理

  1. temperaturewas heated for 24 hours
  2. temperatureUpon cooling the mixture
  3. customwas evaporated
  4. dissolutionThe residue was dissolved in methylene chloride
  5. washwashed with water
  6. dry with materialwith saturated NaCl solution, dried over magnesium sulfate
  7. filtrationfiltered
  8. customThe filtrate was evaporated
  9. customrecrystallized several times from methanol-diethyl ether

出典と根拠

ORDレコード
ord-ff9402944aff491a8a73dbf5e8c9d32d
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03957988

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