Hydrogen Sulfide → HCID 14950598、化合物

HRID 357622ノート

反応式

HRID 357622 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 14950598HCID 14950598、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-101305402571408cb31c9881afa6b2f7
出典データセット
uspto-grants-1998_11
特許番号
US05840911

反応ノート

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