Sodium Hydroxide → Gsk-269984A

HRID 2356613

反応式

HRID 2356613 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=2[F:29])=[C:6]([CH2:8][C:9]2[N:14]=[C:13]([C:15]([O:17]CC)=[O:16])[CH:12]=[CH:11][CH:10]=2)[CH:7]=1.[OH-].[Na+:31]>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=2[F:29])=[C:6]([CH2:8][C:9]2[N:14]=[C:13]([C:15]([O-:17])=[O:16])[CH:12]=[CH:11][CH:10]=2)[CH:7]=1.[Na+:31]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 59384237Ethyl 6-(5-chloro-2-((4-chloro-2-fluorobenzyl)oxy)benzyl)picolinate

生成物 1

HCID 23696973Gsk-269984A

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

117 g (0.27 mol) of ethyl 6-[(5-chloro-2-{[(4-chloro-2-fluorophenyl)methyl]oxy}phenyl)-methyl]-2-pyridinecarboxylate were dissolved in ethanol (1 litre) (heating required) and 2M sodium hydroxide (200 ml) was added while still hot. Left to crystallise, and when at room temperature was diluted with an equal volume of water. After one hour at room temperature the solid was filtered off and washed with ethanol/water (1:3). MLS (mother liquors) were evaporated to remove ethanol, the solid was filtered off and the two lots were combined and washed with water and ether. Dried in a vacuum oven for 16 hours at 40° C. and 3 days at 60° C. Yield 110.5 g.

後処理

  1. waitLeft
  2. customto crystallise
  3. additionwhen at room temperature was diluted with an equal volume of water
  4. filtrationAfter one hour at room temperature the solid was filtered off
  5. washwashed with ethanol/water (1:3)
  6. customMLS (mother liquors) were evaporated
  7. customto remove ethanol
  8. filtrationthe solid was filtered off
  9. washwashed with water and ether
  10. customDried in a vacuum oven for 16 hours at 40° C. and 3 days at 60° C

出典と根拠

ORDレコード
ord-08e2f34df64749dcae11d5a7e9596421
出典データセット
uspto-grants-2010_07
特許番号
US07759369B2

関連ノート

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