ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Ethanolamine → methanesulfonic acid 8-fluoro-5-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-5H-6-thia-chrysen-2-yl ester

HRID 1513942
ノート
印刷プレビュー

反応式

HRID 1513942 の反応式
C1(C(C2C=CC=CC=2)([C@@H]2CCCN2)O)C=CC=CC=1.B.[F:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]2[C:29]([C:43](=O)[C:44]3[CH:49]=[CH:48][C:47]([O:50][CH2:51][CH2:52][N:53]4[CH2:58][CH2:57][CH2:56][CH2:55][CH2:54]4)=[CH:46][CH:45]=3)=[C:30]3[C:35](=[CH:36][CH:37]=2)[CH:34]=[C:33]([O:38][S:39]([CH3:42])(=[O:41])=[O:40])[CH:32]=[CH:31]3)=[C:24]([S:60]C)[CH:23]=1.C(CN)O.[Cl-].[NH4+].C(N(CC)CC)C.CS(Cl)(=O)=O.C(=O)(O)[O-].[Na+]>C1COCC1>[F:21][C:22]1[CH:23]=[C:24]2[C:25](=[CH:26][CH:27]=1)[C:28]1[C:29](=[C:30]3[C:35](=[CH:36][CH:37]=1)[CH:34]=[C:33]([O:38][S:39]([CH3:42])(=[O:40])=[O:41])[CH:32]=[CH:31]3)[CH:43]([C:44]1[CH:45]=[CH:46][C:47]([O:50][CH2:51][CH2:52][N:53]3[CH2:58][CH2:57][CH2:56][CH2:55][CH2:54]3)=[CH:48][CH:49]=1)[S:60]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 8

HCID 700EthanolamineHCID 6331Borane2 回HCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 31297Methanesulfonyl chloride2 回HCID 516892Sodium BicarbonateHCID 27248992-Pyrrolidinemethanol, alpha,alpha-diphenyl-, (S)-
HCID 11238709
Methanesulfonic acid 6-(4-fluoro-2-methylsulfanyl-phenyl)-5-[4-(2-piperidin-1-yl-ethoxy)-benzoyl]-naphthalen-2-yl ester

生成物 1

HCID 11249977methanesulfonic acid 8-fluoro-5-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-5H-6-thia-chrysen-2-yl ester収率 88.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
45 °C

実験手順

Charge a flask with (s)-(−)-α,α-diphenyl-2-pyrrolidinemethanol (380 mg, 1.5 mmol), dissolve with 1M borane in THF (60 mL, 60 mmol), purge with nitrogen and heat to 45° C. Dissolve methanesulfonic acid 6-(4-fluoro-2-methylsulfanyl-phenyl)-5-[4-(2-piperidin-1-yl-ethoxy)-benzoyl]-naphthalen-2-yl ester (9.0 g, 15.1 mmol) in dry THF (80 mL) and add to the borane solution via syringe pump over 2 hours. After the addition is complete, add ethanolamine (18.2 mL, 300 mmol) and stir at 45° C. for 3 hours. Pour the reaction into saturated aqueous ammonium chloride and extract with methylene chloride. Dry over sodium sulfate, filter and concentrate to a beige foam. Dissolve the crude foam in dry THF (150 mL). Add triethylamine (12.4 mL, 90 mmol) and methanesulfonyl chloride (7.0 mL, 90 mmol) and heat to reflux under nitrogen. Add more methanesulfonyl chloride (0.45 mL, 5.8 mmol) after 2 hours to drive the reaction to completion. Pour the reaction into saturated aqueous sodium bicarbonate and extract twice with methylene chloride. Dry the combined organic layers with sodium sulfate, filter and concentrate. Purify the residue on silica gel (0% to 4% methanol in methylene chloride) to yield 7.5 g (88%) of the title compound. HPLC Rt (0.01% heptafluorobutyric acid:1.0% isopropylalcohol:water is mobile phase A and 0.01% heptafluorobutyric acid:1.0% isopropylalcohol:acetonitrile is mobile phase B; gradient method 25 to 95% B, Purity@254 nm)=2.96 min (100%); mass spectrum (ion spray): m/z=564.3 (M+H).

後処理

  1. custompurge with nitrogen
  2. additionAfter the addition
  3. additionPour
  4. extractionextract with methylene chloride
  5. dry with materialDry over sodium sulfate
  6. filtrationfilter
  7. concentrationconcentrate to a beige foam
  8. dissolutionDissolve the crude foam in dry THF (150 mL)
  9. temperatureto reflux under nitrogen
  10. customthe reaction to completion
  11. additionPour
  12. extractionextract twice with methylene chloride
  13. dry with materialDry the combined organic layers with sodium sulfate
  14. filtrationfilter
  15. concentrationconcentrate
  16. customPurify the residue on silica gel (0% to 4% methanol in methylene chloride)

出典と根拠

ORDレコード
ord-92ba206267a5437dbfe0cbe273e0c9fe
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217032B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート