Hydrochloric Acid → HCID 20161182, 화합물

HRID 247018노트

반응식

HRID 247018 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[CH2:8][C:7]([C:14]#N)=[CH:6]2.[H-].C([Al+]CC(C)C)C(C)C.C[OH:27].Cl>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[CH2:8][C:7]([CH:14]=[O:27])=[CH:6]2

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 20161200HCID 20161200, 화합물HCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 20161182HCID 20161182, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
-5 °C

실험 절차

5,6-Dimethoxy-1H-indene-2-carbonitrile (1.8 g) was suspended in dry toluene (40 ml) under an atmosphere of nitrogen. The reaction mixture was cooled to -5° C. and treated dropwise with a solution of diisobutylaluminium hydride in toluene (1.5M, 13 ml). After 30 minutes the solution was treated with methanol (5 ml) then poured into hydrochloric acid (1M, 200 ml) and stirred for 15 minutes. The resultant solution was extracted into dichloromethane (4×100 ml) then the organic extracts were combined, washed with brine, dried over magnesium sulphate and evaporated to dryness. The residue (1.4 g) was crystallised from dichloromethane:ether to give 5,6-dimethoxy-1-H-indene-2-carboxaldehyde as a white solid, m.p. 125°-128° C.

후처리

  1. extractionThe resultant solution was extracted into dichloromethane (4×100 ml)
  2. washwashed with brine
  3. dry with materialdried over magnesium sulphate
  4. customevaporated to dryness
  5. customThe residue (1.4 g) was crystallised from dichloromethane

출처 및 근거

ORD 기록
ord-09f438ec31564fc782eae76b2e281f46
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705782

반응 노트

불러오는 중…