Sodium Hydroxide → Sodium 5-(4-{1-[({2,5-dimethyl-4-[4-(trifluoromethyl)benzyl]-3-thienyl}carbonyl)amino]cyclopropyl}phenyl)tetrazol-2-ide

HRID 870064ノート

反応式

HRID 870064 の反応式
[CH3:1][C:2]1[S:3][C:4]([CH3:35])=[C:5]([CH2:24][C:25]2[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[CH:27][CH:26]=2)[C:6]=1[C:7]([NH:9][C:10]1([C:13]2[CH:18]=[CH:17][C:16]([C:19]3[N:20]=[N:21][NH:22][N:23]=3)=[CH:15][CH:14]=2)[CH2:12][CH2:11]1)=[O:8].[OH-].[Na+:37]>CCO>[CH3:1][C:2]1[S:3][C:4]([CH3:35])=[C:5]([CH2:24][C:25]2[CH:26]=[CH:27][C:28]([C:31]([F:34])([F:32])[F:33])=[CH:29][CH:30]=2)[C:6]=1[C:7]([NH:9][C:10]1([C:13]2[CH:18]=[CH:17][C:16]([C:19]3[N:20]=[N:21][N-:22][N:23]=3)=[CH:15][CH:14]=2)[CH2:11][CH2:12]1)=[O:8].[Na+:37]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 249529282,5-Dimethyl-N-{1-[4-(2H-tetrazol-5-yl)phenyl]cyclopropyl}-4-[4-(trifluoromethyl)benzyl]thiophene-3-carboxamide

生成物 1

HCID 24953973Sodium 5-(4-{1-[({2,5-dimethyl-4-[4-(trifluoromethyl)benzyl]-3-thienyl}carbonyl)amino]cyclopropyl}phenyl)tetrazol-2-ide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of 2,5-dimethyl-N-{1-[4-(2H-tetrazol-5-yl)phenyl]cyclopropyl}-4-[4-(trifluoromethyl)benzyl]thiophene-3-carboxamide from Example 14, Step 3 (150 mg, 0.301 mmol) in EtOH (3 mL), was treated with NaOH (1.0N in water, 301 μL, 0.301 mmol). The solution then obtained was concentrated to dryness. Water (20 mL) was added to the residue. The turbid solution was frozen in a bath of dry ice and acetone and lyophilized to afford the desired product as an off-white fluffy solid. MS (−APCI): m/z 496 (M−23)−.

後処理

  1. customThe solution then obtained
  2. concentrationwas concentrated to dryness
  3. additionWater (20 mL) was added to the residue
  4. temperatureThe turbid solution was frozen in a bath of dry ice and acetone

出典と根拠

ORDレコード
ord-4e69e387c7b644fc8251835c1433bd72
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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