Sodium Hydroxide → MK-2894 (sodium salt)

HRID 870068ノート

反応式

HRID 870068 の反応式
[CH3:1][C:2]1[S:3][C:4]([CH3:33])=[C:5]([CH2:22][C:23]2[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:31])[F:30])=[CH:25][CH:24]=2)[C:6]=1[C:7]([NH:9][C:10]1([C:13]2[CH:21]=[CH:20][C:16]([C:17]([OH:19])=[O:18])=[CH:15][CH:14]=2)[CH2:12][CH2:11]1)=[O:8].[OH-].[Na+:35]>CCO>[CH3:1][C:2]1[S:3][C:4]([CH3:33])=[C:5]([CH2:22][C:23]2[CH:24]=[CH:25][C:26]([C:29]([F:31])([F:30])[F:32])=[CH:27][CH:28]=2)[C:6]=1[C:7]([NH:9][C:10]1([C:13]2[CH:21]=[CH:20][C:16]([C:17]([O-:19])=[O:18])=[CH:15][CH:14]=2)[CH2:12][CH2:11]1)=[O:8].[Na+:35]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 24952929MK-2894

生成物 1

HCID 24953972MK-2894 (sodium salt)

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 4-{1-[({2,5-dimethyl-4-[4-(trifluoromethyl)benzyl]-3-thienyl}carbonyl)amino]cyclopropyl}benzoic acid from Example 16, Step 4 (112 mg, 0.236 mmol) in EtOH (5 mL), was treated with NaOH (1.0N in water, 236 μL, 0.236 mmol) after which a precipitate was formed. The mixture then obtained was concentrated to dryness. Water (15 mL) was added to the residue. The very fine resulting suspension was frozen in a bath of dry ice and acetone and lyophilized to afford the desired product as a white fluffy solid. MS (−APCI): m/z 472 (M−23)−.

後処理

  1. customwas formed
  2. customThe mixture then obtained
  3. concentrationwas concentrated to dryness
  4. additionWater (15 mL) was added to the residue
  5. temperatureThe very fine resulting suspension was frozen in a bath of dry ice and acetone

出典と根拠

ORDレコード
ord-3ef53e3cd02d4263bff0dd5e98e907fa
出典データセット
uspto-grants-2015_03
特許番号
US08969394B2

反応ノート

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