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Tributylphosphine → HCID 68419400、化合物

HRID 2356168
ノート
印刷プレビュー

反応式

HRID 2356168 の反応式
[CH2:1]([O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1O)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[Br:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]O.C(P(CCCC)CCCC)CCC.N(C(N1CCCCC1)=O)=NC(N1CCCCC1)=O>CCCCCC.C(Cl)Cl>[Br:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=1[O:7][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]
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 13831TributylphosphineHCID 730421,1'-(Azodicarbonyl)dipiperidineHCID 275701316-Bromo-1-hexadecanolHCID 124137162-(Hexyloxy)phenol

生成物 1

HCID 68419400HCID 68419400、化合物収率 83.4%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回
HCID 8058Hexane溶媒

実験手順

To 350 mL of dehydrated methylene chloride, 12.8 g (66 mmol) of 2-hexyloxyphenol, 23.3 g (73 mmol) of 16-bromohexadecane-1-ol, and 20.0 g (99 mmol) of tri-n-butylphosphine were added. The resulting mixture was cooled with ice under argon. After 25.0 g (99 mmol) of 1,1′-(azodicarbonyl)dipiperidine was added bit by bit while stirring the mixture, 150 mL of methylene chloride was added. Under argon, the mixture was stirred at ambient temperature for 30 minutes and was refluxed for 6 hours. After being cooled, the reaction solution was put into 100 mL of hexane and was filtered. The filtered liquid was purified by silica-gel column chromatography. As a result, 26.5 g of a transparent liquid was obtained.

後処理

  1. temperatureThe resulting mixture was cooled with ice under argon
  2. additionwas added
  3. temperaturewas refluxed for 6 hours
  4. temperatureAfter being cooled
  5. filtrationwas filtered
  6. customThe filtered liquid was purified by silica-gel column chromatography

出典と根拠

ORDレコード
ord-846ddec337684784ae02943f5369d82c
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07758932B2

反応ノート

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