Water → HCID 22136372, 화합물

HRID 2302031노트

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HRID 2302031 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 22136372HCID 22136372, 화합물수율 31.5%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

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온도
70 °C

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-1206f1d11a894dfe8c905ab0f1597d4e
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06429207B1

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