Water → HCID 22136372、化合物

HRID 1826874ノート

反応式

HRID 1826874 の反応式
Cl.[N:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12](Cl)=[O:13])=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1.[C:15]12([OH:25])[CH2:24][CH:19]3[CH2:20][CH:21]([CH2:23][CH:17]([CH2:18]3)[CH2:16]1)[CH2:22]2.O>N1C=CC=CC=1>[N:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12]([O:25][C:15]34[CH2:22][CH:21]5[CH2:20][CH:19]([CH2:18][CH:17]([CH2:23]5)[CH2:16]3)[CH2:24]4)=[O:13])=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 962WaterHCID 641521-AdamantanolHCID 22136358Quinoline-6-carbonyl chloride hydrochloride

生成物 1

HCID 22136372HCID 22136372、化合物収率 31.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

反応条件

温度
70 °C

実験手順

6-Quinolinecarbonyl chloride hydrochloride (0.76 g, 3.3 mmol) in pyridine (2 mL) was added to a solution of 1-adamantanol (0.60 g, 3.9 mmol) in pyridine (8 mL). The reaction was stirred at 70° C. for 16 h. To the stirring reaction mixture was added water (100 mL) which caused the product to precipitate. This precipitate was filtered and then washed with water (3×25 mL). The filter cake was dissolved in ethanol (20 mL) and water was then added to the cloud point (16 mL). The crystallizing solution was allowed to stand for 15 h. Filtering and drying under high vacuum for 7 h provided 0.32 g (26%) of (61) as light brown needle-like crystals:

後処理

  1. customTo the stirring reaction mixture
  2. customto precipitate
  3. filtrationThis precipitate was filtered
  4. washwashed with water (3×25 mL)
  5. dissolutionThe filter cake was dissolved in ethanol (20 mL)
  6. additionwater was then added to the cloud point (16 mL)
  7. waitto stand for 15 h
  8. filtrationFiltering
  9. customdrying under high vacuum for 7 h

出典と根拠

ORDレコード
ord-96bee3001af4484ca83846fc6cd86274
出典データセット
uspto-grants-2006_05
特許番号
US07053104B2

反応ノート

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