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

HRID 887914노트

반응식

HRID 887914 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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-2-carbothioamide (intermediate 13, mp. 194-195° C.).

후처리

  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

출처 및 근거

ORD 기록
ord-cdc65adc94164087acfeb0b9b083e013
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247432B2

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