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Pivaloyl chloride → HCID 18604484、化合物

HRID 64999
ノート
印刷プレビュー

反応式

HRID 64999 の反応式
[BrH:1].[OH:2][C:3]1[C:16]2[CH2:15][CH2:14][C@H:13]3[C@@H:8]([CH2:9][CH2:10][CH2:11][NH:12]3)[C:7]=2[CH:6]=[CH:5][CH:4]=1.[C:17](Cl)(=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19]>FC(F)(F)C(O)=O>[BrH:1].[C:17]([O:2][C:3]1[C:16]2[CH2:15][CH2:14][C@H:13]3[C@@H:8]([CH2:9][CH2:10][CH2:11][NH:12]3)[C:7]=2[CH:6]=[CH:5][CH:4]=1)(=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 62493Pivaloyl chlorideHCID 9882256(+/-)-trans-7-Hydroxy-1,2,3,4,4a,5,6,10b-octahydrobenzo(f)quinoline hydrobromide

生成物 1

HCID 18604484HCID 18604484、化合物

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

(±)-trans-7-Hydroxy-1,2,3,4,4a,5,6,10b-octahydrobenzo(f)quinoline hydrobromide (50 mg, 0.17 mmol) was dissolved in trifluoroacetic acid (1 ml). Pivaloyl chloride (0.2 ml) was added and the mixture was stirred at room temperature overnight. After evaporation of the solvent, the residue was partitioned between H2O and CH2Cl2. The organic layer was concentrated and applied to a SiO2 column and the product was eluted with CH2Cl2 -MeOH. Fractions containing the product were collected. The solvent was evaporated yielding 20 mg of an oil. GC-MS: M+ at m/e 287.

後処理

  1. customAfter evaporation of the solvent
  2. customthe residue was partitioned between H2O and CH2Cl2
  3. concentrationThe organic layer was concentrated
  4. washthe product was eluted with CH2Cl2 -MeOH
  5. additionFractions containing the product
  6. customwere collected
  7. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-fdba1475d808437296ab4bd09fdf9cde
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04612316

反応ノート

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