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Potassium Iodide → 9-[8-(2,2,2-Trifluoroacetyl)-8-aza-bicyclo[3.2.1]oct-3-yl]-9H-xanthene-3-carbonitrile

HRID 733409
ノート
印刷プレビュー

反応式

HRID 733409 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]2[CH:6]([CH:16]3[CH2:22][CH:21]4[N:23]([C:24](=[O:29])[C:25]([F:28])([F:27])[F:26])[CH:18]([CH2:19][CH2:20]4)[CH2:17]3)[C:7]3[C:12]([O:13][C:14]=2[CH:15]=1)=[CH:11][CH:10]=[CH:9][CH:8]=3.[Cu](C#N)[C:31]#[N:32].[I-].[K+]>CN(C=O)C>[F:27][C:25]([F:26])([F:28])[C:24]([N:23]1[CH:21]2[CH2:20][CH2:19][CH:18]1[CH2:17][CH:16]([CH:6]1[C:5]3[CH:4]=[CH:3][C:2]([C:31]#[N:32])=[CH:15][C:14]=3[O:13][C:12]3[C:7]1=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:22]2)=[O:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 4875Potassium IodideHCID 578392651-[3-(3-Bromo-9H-xanthen-9-yl)-8-aza-bicyclo[3.2.1]oct-8-yl]-2,2,2-trifluoroethanone2 回HCID 178418260HCID 178418260、化合物2 回

生成物 1

HCID 578392559-[8-(2,2,2-Trifluoroacetyl)-8-aza-bicyclo[3.2.1]oct-3-yl]-9H-xanthene-3-carbonitrile収率 60%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 1-[3-(3-bromo-9H-xanthen-9-yl)-8-aza-bicyclo[3.2.1]oct-8-yl]-2,2,2-trifluoro-ethanone, 2j (1.8 g, 3.86 mmol) in DMF (40 mL) was added copper cyanide (0.69 g, 7.72 mmol) and potassium iodide (50 mg), and the mixture was heated to reflux for 18 h. More copper cyanide (0.43 g) was added, and the mixture was heated to reflux for 30 h. The mixture was filtered and poured in ice-water. The solid was separated via filtration, washed with water, and air-dried. The crude product was purified via flash column chromatography (eluent gradient: 5% to 30% ethyl acetate in heptane) to yield 0.956 g (60%) of title compound 9-[8-(2,2,2-trifluoroacetyl)-8-aza-bicyclo[3.2.1]oct-3-yl]-9H-xanthene-3-carbonitrile, 3j. MS m/z (MH+) 412.8.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 18 h
  3. temperaturethe mixture was heated
  4. temperatureto reflux for 30 h
  5. filtrationThe mixture was filtered
  6. additionpoured in ice-water
  7. customThe solid was separated via filtration
  8. washwashed with water
  9. customair-dried
  10. customThe crude product was purified via flash column chromatography (eluent gradient: 5% to 30% ethyl acetate in heptane)

出典と根拠

ORDレコード
ord-86cce731f2f14898ae6c4fbfc5930a8a
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07589104B2

反応ノート

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