Thionyl Chloride → 4-(4-Benzyloxy-3-chloromethylphenoxy)-5-methyl-7-nitroindane

HRID 1766650ノート

反応式

HRID 1766650 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][C:16]2[C:24]([CH3:25])=[CH:23][C:22]([N+:26]([O-:28])=[O:27])=[C:21]3[C:17]=2[CH2:18][CH2:19][CH2:20]3)=[CH:11][C:10]=1[CH2:29]O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:33])=O>C(OCC)C>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][C:16]2[C:24]([CH3:25])=[CH:23][C:22]([N+:26]([O-:28])=[O:27])=[C:21]3[C:17]=2[CH2:18][CH2:19][CH2:20]3)=[CH:11][C:10]=1[CH2:29][Cl:33])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 23031098[2-Benzyloxy-5-(5-methyl-7-nitroindan-4-yloxy)phenyl]methanol

生成物 1

HCID 230311674-(4-Benzyloxy-3-chloromethylphenoxy)-5-methyl-7-nitroindane

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

[2-benzyloxy-5-(5-methyl-7-nitroindan-4-yloxy)phenyl]methanol (2.48 g) was dissolved in diethyl ether. After adding dropwise thionyl chloride (5 mL) under ice-cooling with stirring, the mixture was stirred at room temperature for 6 hours. The reaction mixture was evaporated under reduced pressure to dryness. After adding water (10 mL), the residue was extracted with diethyl ether. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the title compound (2.04 g).

後処理

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 6 hours
  3. customThe reaction mixture was evaporated under reduced pressure to dryness
  4. additionAfter adding water (10 mL)
  5. extractionthe residue was extracted with diethyl ether
  6. washThe organic layer was washed with brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-0580df68c11b4842a5f286b946988595
出典データセット
uspto-grants-2007_06
特許番号
US07230031B2

反応ノート

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