Thionyl Chloride → Methyl 1-chloroindan-4-carboxylate

HRID 1763422

反応式

HRID 1763422 の反応式
O[CH:2]1[C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([C:11]([O:13][CH3:14])=[O:12])[C:5]=2[CH2:4][CH2:3]1.S(Cl)([Cl:17])=O>C(Cl)(Cl)Cl>[Cl:17][CH:2]1[C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([C:11]([O:13][CH3:14])=[O:12])[C:5]=2[CH2:4][CH2:3]1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 20310103Methyl 1-hydroxyindan-4-carboxylate

生成物 1

HCID 20310089Methyl 1-chloroindan-4-carboxylate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

In 6 ml. of chloroform is dissolved 5.7 g. of methyl 1-hydroxyindan-4-carboxylate and, under cooling with ice, the solution is stirred. Then, 3 ml. of thionyl chloride is added dropwise and, after the dropwise addition has been completed, the mixture is further stirred under cooling with ice for one hour. Then, the solvent and the excess thionyl chloride are distilled off under reduced pressure. The residue obtained is purified by column chromatography on silica gel (500 g. silica gel; eluant: chloroform). The procedure gives methyl 1-chloroindan-4-carboxylate as an oily product.

後処理

  1. additionafter the dropwise addition
  2. stirringthe mixture is further stirred
  3. temperatureunder cooling with ice for one hour
  4. distillationThen, the solvent and the excess thionyl chloride are distilled off under reduced pressure
  5. customThe residue obtained
  6. customis purified by column chromatography on silica gel (500 g. silica gel; eluant: chloroform)

出典と根拠

ORDレコード
ord-5c52c6d286014d4bb5165b68d9ff3572
出典データセット
uspto-grants-1978_09
特許番号
US04111997

関連ノート

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