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Dimethylamine → N-((1R,2S)-1-(1-(4-((dimethylamino)methyl)phenyl)-1H-indazol-5-yloxy)-1-phenylpropan-2-yl)-2,2,2-trifluoroacetamide

HRID 1098940
ノート
印刷プレビュー

反応式

HRID 1098940 の反応式
[F:1][C:2]([F:34])([F:33])[C:3]([NH:5][C@@H:6]([CH3:32])[C@H:7]([O:14][C:15]1[CH:16]=[C:17]2[C:21](=[CH:22][CH:23]=1)[N:20]([C:24]1[CH:29]=[CH:28][C:27]([CH2:30]O)=[CH:26][CH:25]=1)[N:19]=[CH:18]2)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:4].[CH2:35]([N:37](CC)[CH2:38]C)C.CS(Cl)(=O)=O.CNC>[Cl-].[Na+].O.ClCCl>[CH3:35][N:37]([CH2:30][C:27]1[CH:26]=[CH:25][C:24]([N:20]2[C:21]3[C:17](=[CH:16][C:15]([O:14][C@H:7]([C:8]4[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=4)[C@@H:6]([NH:5][C:3](=[O:4])[C:2]([F:34])([F:33])[F:1])[CH3:32])=[CH:23][CH:22]=3)[CH:18]=[N:19]2)=[CH:29][CH:28]=1)[CH3:38]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 674DimethylamineHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 59339791HCID 59339791、化合物

生成物 1

HCID 59339629N-((1R,2S)-1-(1-(4-((dimethylamino)methyl)phenyl)-1H-indazol-5-yloxy)-1-phenylpropan-2-yl)-2,2,2-trifluoroacetamide

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 57417360Sodium chloride; water溶媒

実験手順

To a stirred, ice-cooled suspension of 2,2,2-trifluoro-N-((1R,2S)-1-(1-(4-(hydroxymethyl)phenyl)-1H-indazol-5-yloxy)-1-phenylpropan-2-yl)acetamide (141, 118 mg, 0.25 mmol) and triethylamine (0.35 mL, 2.5 mmol) was added methanesulfonyl chloride (140 μL, 1.8 mmol). After stirring for 50 min at 0° C. brine and dichloromethane (10 mL) were added. The mixture was washed with aqueous KHSO4 (1M) and sat. aqueous NaHCO3. To the organic phase was added dimethylamine (0.75 mL, 11.3 mmol). The mixture was stirred at ambient temperature for 40 min and was then evaporated. Preparative HPLC (Kromasil C-18, 2.5×20 cm, 30-90% CH3CN in water/40 min (0.1% TfA) afforded slightly impure title compound as a TfA-salt. The material was dissolved in MeOH and absorbed on a plug of acidic ion exchange resin (SCX, 5 g, pre-washed with MeOH). Eluting subsequently with MeOH and methanolic ammonia (2M) gave somewhat impure title compound. Purification by preparative HPLC on an XBridge C-18 column using a gradient of 50-90% acetonitrile in water containing 0.1% aqueous ammonia (28%). afforded pure N-((1R,2S)-1-(1-(4-((dimethylamino)methyl)phenyl)-1H-indazol-5-yloxy)-1-phenylpropan-2-yl)-2,2,2-trifluoroacetamide (77 mg, 61%).

後処理

  1. temperatureTo a stirred, ice-cooled
  2. additionwere added
  3. washThe mixture was washed with aqueous KHSO4 (1M) and sat. aqueous NaHCO3
  4. customwas then evaporated

出典と根拠

ORDレコード
ord-ec01064a3fef43acbc3f770203bdbcbc
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08143290B2

反応ノート

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