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Ammonium → HCID 57471474、化合物

HRID 2177130
ノート
印刷プレビュー

反応式

HRID 2177130 の反応式
Cl[C:2]1[CH:3]=[C:4]([CH:30]=[CH:31][CH:32]=1)[CH2:5][CH:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([CH2:16][CH2:17][S:18]([CH2:21][CH2:22][CH3:23])(=O)=O)[CH:14]=2)[CH2:9][CH2:8][CH:7]1[NH:24][C:25](=[O:29])[O:26][CH2:27][CH3:28].[NH4+]>CO.[Pd]>[CH2:27]([O:26][C:25](=[O:29])[NH:24][CH:7]1[CH2:8][CH2:9][C:10]2[C:15](=[CH:14][C:13]([CH2:16][CH2:17][S:18][CH2:21][CH2:22][CH3:23])=[CH:12][CH:11]=2)[CH:6]1[CH2:5][C:4]1[CH:3]=[CH:2][CH:32]=[CH:31][CH:30]=1)[CH3:28]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 223AmmoniumHCID 57471473HCID 57471473、化合物

生成物 1

HCID 57471474HCID 57471474、化合物収率 54.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

反応条件

温度
80 °C

実験手順

Ethyl 1-(3-chlorobenzyl)-7-(2-(propylsulfonyl)ethyl)-1,2,3,4-tetrahydronaphthalen-2-ylcarbamate (27.1 mg, 0.057 mmol) and ammonium form late (71.5 mg, 1.134 mmol) were dissolved in 5 ml MeOH. Pd/C (0.845 mg, 7.94 μmol) was added and stirred at 80° C. for 4 h. The mixture was filtered, the solvent evaporated, the residue re-dissolved in ethyl acetate, which was subsequently washed with water, NaHCO3 and brine, dried, filtered. Solvent was evaporated to obtain white solid which was purified by chromatography affording 12.7 mg of product as a white solid.

後処理

  1. filtrationThe mixture was filtered
  2. customthe solvent evaporated
  3. dissolutionthe residue re-dissolved in ethyl acetate
  4. washwhich was subsequently washed with water, NaHCO3 and brine
  5. customdried
  6. filtrationfiltered
  7. customSolvent was evaporated
  8. customto obtain white solid which
  9. customwas purified by chromatography

出典と根拠

ORDレコード
ord-fa90a9f0bb50422aba8d6aae6cd1fe2f
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09067871B2

反応ノート

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