Sodium Hydroxide → MK-2894 (sodium salt)

HRID 870068노트

반응식

HRID 870068 반응식
[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]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 24952929MK-2894

생성물 1

HCID 24953972MK-2894 (sodium salt)

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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)−.

후처리

  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

출처 및 근거

ORD 기록
ord-3ef53e3cd02d4263bff0dd5e98e907fa
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969394B2

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