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

Tetrahydrofuran → 2-[(S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethoxy]-N-(2,2,3,3,3-pentafluoropropyl)acetamide

HRID 1922623
ノート
印刷プレビュー

反応式

HRID 1922623 の反応式
C[Si](C)(C)[N-][Si](C)(C)C.[Na+].O1CCCC1.[Br:16]/[CH:17]=[C:18]1\[CH2:19][CH2:20][CH2:21][C@@:22]2([CH3:30])[C@H:26]\1[CH2:25][CH:24]=[C:23]2[C@@H:27]([OH:29])[CH3:28].Br[CH2:32][C:33]([NH:35][CH2:36][C:37]([F:43])([F:42])[C:38]([F:41])([F:40])[F:39])=[O:34].[Cl-].[NH4+]>CN(C)C=O.CCCCCC>[Br:16]/[CH:17]=[C:18]1\[CH2:19][CH2:20][CH2:21][C@@:22]2([CH3:30])[C@H:26]\1[CH2:25][CH:24]=[C:23]2[C@@H:27]([O:29][CH2:32][C:33]([NH:35][CH2:36][C:37]([F:42])([F:43])[C:38]([F:41])([F:39])[F:40])=[O:34])[CH3:28]
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

8

反応物 5

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 2724254Sodium bis(trimethylsilyl)amideHCID 59456520(S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethanol2 回HCID 594565462-bromo-N-(2,2,3,3,3-pentafluoropropyl)acetamide

生成物 1

HCID 24746036
2-[(S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethoxy]-N-(2,2,3,3,3-pentafluoropropyl)acetamide

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8058Hexane溶媒

反応条件

温度
-15 °C

実験手順

Under a nitrogen atmosphere, a solution of sodium hexamethyldisilazide in tetrahydrofuran (1.1 M, 5.31 ml, 5.84 mmol) was cooled to −15° C., and a solution of (S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethanol (Compound 5: 633.7 mg, 2.337 mmol) in dimethylformamide (1 ml) was added thereto over 4 minutes. The resulting mixture was stirred at −15° C. for 7 minutes, and a solution of 2-bromo-N-(2,2,3,3,3-pentafluoropropyl)acetamide (726 mg, 2.688 mmol) in dimethylformamide (1 ml) was added thereto over 5 minutes. After stirring the reaction solution at −5° C. for 30 minutes, aqueous ammonium chloride solution (5 ml) and hexane (20 ml) were added thereto, and the separation of the solution was conducted. The obtained organic layer was sequentially washed with water (5 ml) and saturated brine (4 ml)/water (1 ml), and the solvent was evaporated. The obtained crude product was purified by silica gel column chromatography to obtain 2-[(S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethoxy]-N-(2,2,3,3,3-pentafluoropropyl)acetamide (1.08 g, quantitatively).

後処理

  1. waitover 5 minutes
  2. stirringAfter stirring the reaction solution at −5° C. for 30 minutes
  3. customthe separation of the solution
  4. washThe obtained organic layer was sequentially washed with water (5 ml) and saturated brine (4 ml)/water (1 ml)
  5. customthe solvent was evaporated
  6. customThe obtained crude product
  7. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-89a0867db7f64800aea355d36476c984
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08173824B2

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