Hydrochloric Acid → HCID 21986517, 화합물

HRID 9690

반응식

HRID 9690 반응식
[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]

참가 물질

4

반응물 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]benzonitrile2회

생성물 1

HCID 21986517HCID 21986517, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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+.

후처리

  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+

출처 및 근거

ORD 기록
ord-8b8bdbd070704040b63b19183de9bb48
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091237B2

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