Hydrochloric Acid → 3,5,6,7-tetrahydro-s-indacen-1(2H)-one

HRID 1276538ノート

反応式

HRID 1276538 の反応式
Cl[CH2:2][CH2:3][C:4]([C:6]1[CH:7]=[C:8]2[C:12](=[CH:13][CH:14]=1)[CH2:11][CH2:10][CH2:9]2)=[O:5].Cl>S(=O)(=O)(O)O>[C:4]1(=[O:5])[C:6]2[C:14](=[CH:13][C:12]3[CH2:11][CH2:10][CH2:9][C:8]=3[CH:7]=2)[CH2:2][CH2:3]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 32867585-(3-Chloropropionyl)indan

生成物 1

HCID 109318913,5,6,7-tetrahydro-s-indacen-1(2H)-one

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

Concentrated sulfuric acid (550 mL) was added dropwise, with stirring over a time period of 2 hours to 137 grams of 3-chloro-1-indan-5-yl-propan-1-one. The resulting thick black solution was heated to 90° C. until hydrogen chloride evolution ceased (usually 1-4 hours). The mixture was then cooled to room temperature and poured onto 5 kg of ice. The resulting slurry was stirred overnight and filtered. The solid was washed with water until the water ran clear through the filter. The tan solid was then dried in vacuo and recrystallized from hexane to afford 90 grams of the title compound, m.p. 72.4-74.8° C.

後処理

  1. customusually 1-4 hours
  2. filtrationfiltered
  3. washThe solid was washed with water until the water
  4. customThe tan solid was then dried in vacuo
  5. customrecrystallized from hexane

出典と根拠

ORDレコード
ord-90427445a225400eab23a52895d3c9a0
出典データセット
uspto-grants-2000_12
特許番号
US06166064

反応ノート

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