Hydrogen Sulfide → HCID 14950598, 화합물

HRID 357622노트

반응식

HRID 357622 반응식
[C:1]([C:3]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:4]=1[CH2:5][CH2:6][C:7]2=[O:12])#[N:2].C(N(CC)CC)C.[SH2:20]>N1C=CC=CC=1>[C:1]([C:3]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:4]=1[CH2:5][CH2:6][C:7]2=[O:12])(=[S:20])[NH2:2]

참가 물질

5

반응물 3

HCID 402Hydrogen SulfideHCID 8471TriethylamineHCID 27515831-Oxo-2,3-Dihydro-1H-Indene-4-Carbonitrile

생성물 1

HCID 14950598HCID 14950598, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 12.1 g (77 mmol) of 4-cyano-2,3-dihydro-1H-inden-1-one [see Coll. Czechoslov. Chem. Commun. 4, 3227 (1978)] in 220 ml of pyridine and 10.6 ml (77 mmol) of triethylamine is saturated with hydrogen sulfide for 3 hours at 40° and is then stirred at the same temperature for 16 hours. The reaction mixture is cooled and then concentrated to dryness by evaporation, and 300 ml of water are added to the residue. The yellow product that has crystallized out is filtered off with suction, washed with water, dried and recrystallized from ethyl acetate. In that manner there is obtained the title compound, m.p. 197° (decomp.).

후처리

  1. temperatureThe reaction mixture is cooled
  2. concentrationconcentrated to dryness by evaporation, and 300 ml of water
  3. additionare added to the residue
  4. customThe yellow product that has crystallized out
  5. filtrationis filtered off with suction
  6. washwashed with water
  7. customdried
  8. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-101305402571408cb31c9881afa6b2f7
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840911

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