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

HRID 1276538노트

반응식

HRID 1276538 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-90427445a225400eab23a52895d3c9a0
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06166064

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