Hydrochloric Acid → HCID 21986517、化合物

HRID 9690

反応式

HRID 9690 の反応式
[F:1][C:2]1[CH:9]=[C:8]([C:10]2[S:11][C:12]([CH2:16][CH2:17][C:18]3[CH:23]=[CH:22][C:21]([O:24][CH2:25][C:26]45OCC(C)(C[O:31]4)C[O:27]5)=[C:20]([CH3:35])[CH:19]=3)=[C:13]([CH3:15])[CH:14]=2)[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].Cl>CC(O)C>[C:4]([C:3]1[CH:6]=[CH:7][C:8]([C:10]2[S:11][C:12]([CH2:16][CH2:17][C:18]3[CH:23]=[CH:22][C:21]([O:24][CH2:25][C:26]([OH:31])=[O:27])=[C:20]([CH3:35])[CH:19]=3)=[C:13]([CH3:15])[CH:14]=2)=[CH:9][C:2]=1[F:1])#[N:5]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 219863002-Fluoro-4-[4-methyl-5-(2-{3-methyl-4-[(4-methyl-2,6,7-trioxabicyclo[2.2.2]oct-1-yl)methoxy]phenyl}ethyl)thien-2-yl]benzonitrile2 回

生成物 1

HCID 21986517HCID 21986517、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 2-fluoro-4-[4-methyl-5-(2-{3-methyl-4-[(4-methyl-2,6,7-trioxabicyclo[2.2.2]oct-1-yl)methoxy]phenyl}ethyl)thien-2-yl]benzonitrile (intermediate 101, 0.016 g) in 2-propanol (2 ml) was treated with 2M aqueous hydrochloric acid (1 ml) and the mixture stirred at reflux for 2 hours. The solvent was removed and the residue dissolved in 1,4-dioxane (2 ml) and water (1 ml). This mixture was treated with 2M aqueous sodium hydroxide (0.5 ml) and the mixture stirred for 16 hours). The solvent was removed and the residue purified by SPE (aminopropyl). The title compound, as the free acid, was recovered by treating a solution of this product with Dowex H+.

後処理

  1. temperatureat reflux for 2 hours
  2. customThe solvent was removed
  3. dissolutionthe residue dissolved in 1,4-dioxane (2 ml)
  4. additionThis mixture was treated with 2M aqueous sodium hydroxide (0.5 ml)
  5. stirringthe mixture stirred for 16 hours)
  6. customThe solvent was removed
  7. customthe residue purified by SPE (aminopropyl)
  8. customThe title compound, as the free acid, was recovered
  9. additionby treating a solution of this product with Dowex H+

出典と根拠

ORDレコード
ord-8b8bdbd070704040b63b19183de9bb48
出典データセット
uspto-grants-2006_08
特許番号
US07091237B2

関連ノート

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