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Monobenzone → HCID 20645779、化合物

HRID 324152
ノート
印刷プレビュー

反応式

HRID 324152 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:16][C@H:17]([C:26](O)=[O:27])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].C1CCC(N=C=NC2CCCCC2)CC1>ClCCl>[CH3:16][C@H:17]([C:26]([O:15][C:12]1[CH:11]=[CH:10][C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:14][CH:13]=1)=[O:27])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]
参加物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 7638MonobenzoneHCID 10868DicyclohexylcarbodiimideHCID 11063144(S)-1-methylnonylcarboxylic acid

生成物 1

HCID 20645779HCID 20645779、化合物収率 87%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

{circle around (1)}: A mixture comprising 2.00 g of 4-benzyloxyphenol, 1.86 g of (S)-1-methylnonylcarboxylic acid, 2.06 g of DCC and 20 g of dichloromethane was stirred at room temperature for 30 minutes. Then, a catalytic amount of 4-N,N-dimethylaminopyridine was added to the mixture, and the mixture was further stirred at room temperature for 12 hours. After finishing the reaction, insoluble substances were filtered off, followed by distilling off dichloromethane from the filtrate. The resultant residue was purified by means of silica gel column chromatography, whereby 3.2 g of (S)-4-(1′-methylnonylcarbonyloxy)-1-benzyloxybenzene was obtained.

後処理

  1. stirringthe mixture was further stirred at room temperature for 12 hours
  2. customthe reaction, insoluble substances
  3. filtrationwere filtered off
  4. distillationby distilling off dichloromethane from the filtrate
  5. customThe resultant residue was purified by means of silica gel column chromatography

出典と根拠

ORDレコード
ord-2882d96fd87c445d98ec9f07cda9d41a
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06217793B1

反応ノート

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