Hydrogen Sulfide → 1-Acetyl-2,3-dihydro-1H-indole-2-carbothioamide

HRID 1246194ノート

反応式

HRID 1246194 の反応式
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6][CH:5]1[C:13]#[N:14])(=[O:3])[CH3:2].C(N(CC)CC)C.[SH2:22]>N1C=CC=CC=1>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6][CH:5]1[C:13](=[S:22])[NH2:14])(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 402Hydrogen SulfideHCID 8471TriethylamineHCID 148193141-Acetyl-2,3-dihydro-1H-indole-2-carbonitrile

生成物 1

HCID 219141121-Acetyl-2,3-dihydro-1H-indole-2-carbothioamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 1-acetyl-2,3-dihydro-1H-indole-2-carbonitrile (0.00988 mol) and Triethylamine (0.0197 mol) in pyridine (50 ml) was treated with hydrogen sulfide (gas) at room temperature via a bubbler for 2 hours and the resultant saturated reaction mixture was closed and allowed to set for 16 hours. The reaction mixture was poured into 200 ml of an ice water slurry. A voluminous precipitate formed. The mixture was recooled in an ice bath and the precipitate was collected by suction filtration, washed with cold water, and air dried, yielding 1.62 g of 1-acetyl-2,3-dihydro-1H-indole-2carbothioamide (intermediate 13, mp. 194–195° C.).

後処理

  1. customthe resultant saturated reaction mixture was closed
  2. customA voluminous precipitate formed
  3. customThe mixture was recooled in an ice bath
  4. filtrationthe precipitate was collected by suction filtration
  5. washwashed with cold water, and air
  6. customdried

出典と根拠

ORDレコード
ord-5d0761cc03974dafb0fa7dbafb9be578
出典データセット
uspto-grants-2006_10
特許番号
US07125891B2

反応ノート

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