HCID 20161193, 화합물 → HCID 20161200, 화합물

HRID 247017노트

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HRID 247017 반응식
O[C:2]1([C:15]#[N:16])[CH2:10][C:9]2[C:4](=[CH:5][C:6]([O:13][CH3:14])=[C:7]([O:11][CH3:12])[CH:8]=2)[CH2:3]1>Cl>[CH3:14][O:13][C:6]1[CH:5]=[C:4]2[C:9](=[CH:8][C:7]=1[O:11][CH3:12])[CH2:10][C:2]([C:15]#[N:16])=[CH:3]2

참가 물질

3

반응물 1

HCID 20161193HCID 20161193, 화합물

생성물 1

HCID 20161200HCID 20161200, 화합물수율 80.3%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
75 °C

실험 절차

The crude alcohol (17.1 g) was suspended in hydrochloric acid (5M, 170 ml) and the mixture was stirred and heated to 75° C. After 30 min. the dark solution was cooled in an ice-bath and the resultant green solid was filtered off and dried at 60° C. The product was dissolved in dichloromethane and the solution was passed through a column of coarse silica (0.2-0.5 mm, Merck, 80 g). The appropriate fractions were combined and evaporated to dryness to give 5,6-dimethoxy-1H-indene-2-carbonitrile (12.6 g), m.p. 140°-141° C.

후처리

  1. temperatureAfter 30 min. the dark solution was cooled in an ice-bath
  2. filtrationthe resultant green solid was filtered off
  3. customdried at 60° C
  4. dissolutionThe product was dissolved in dichloromethane
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-b2e11faffd634216adb7d3266e55c54e
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705782

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