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

Triethylamine → 2-tert-Butyl-4-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-methyl-6-phenyl-1,3-benzoxazole-7-carbonitrile

HRID 17529
ノート
印刷プレビュー

反応式

HRID 17529 の反応式
[C:1]([C:5]1[O:6][C:7]2[C:13]([C:14]#[N:15])=[C:12]([CH3:16])[C:11](C3C=CC=CC=3)=[C:10](F)[C:8]=2[N:9]=1)([CH3:4])([CH3:3])[CH3:2].C(N([CH2:29][CH3:30])CC)C.[CH3:31][N:32]([CH3:38])[C@H:33]1[CH2:37][CH2:36][NH:35][CH2:34]1.C(=O)([O-])O.[Na+]>CS(C)=O.C(OCC)(=O)C>[C:1]([CH:5]1[N:9]=[C:8]2[C:10]([N:35]3[CH2:36][CH2:37][C@H:33]([N:32]([CH3:38])[CH3:31])[CH2:34]3)=[CH:11][C:12]([CH3:16])([C:30]3[CH:29]=[CH:10][CH:8]=[CH:7][CH:13]=3)[C:13]([C:14]#[N:15])=[C:7]2[O:6]1)([CH3:3])([CH3:4])[CH3:2]
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

7

反応物 4

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 7019156(3S)-(-)-3-(Dimethylamino)pyrrolidineHCID 68584886HCID 68584886、化合物

生成物 1

HCID 685848532-tert-Butyl-4-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-methyl-6-phenyl-1,3-benzoxazole-7-carbonitrile収率 87%

試薬・触媒・溶媒 2

HCID 679
Dimethyl Sulfoxide
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

2-tert-Butyl-4-fluoro-6-methyl-5-phenyl-1,3-benzoxazole-7-carbonitrile (I-239) (105 mg, 0.34 mmol) was dissolved in dimethyl sulfoxide (2 ml), and at room temperature, triethylamine (95 μl, 0.68 mmol) and (3S)-3-(dimethylamino)pyrrolidine (65 μl, 0.51 mmol) were added. The solution was stirred under nitrogen atmosphere at 90° C. for 6 hours. After cooling to room temperature, the reaction liquid was fractionated with ethyl acetate and an aqueous saturated sodium hydrogencarbonate solution. The aqueous layer was further extracted with ethyl acetate. The organic layers were combined, washed with saturated brine, then dried over anhydrous sodium sulfate. The insoluble matter was separated by filtration, then the solvent was evaporated away, and the resulting residue was purified by middle-pressure liquid chromatography (eluent, chloroform:methanol=98:2) to obtain the entitled compound (119 mg, 87%) as a pale yellow solid.

後処理

  1. temperatureAfter cooling to room temperature
  2. customthe reaction liquid
  3. extractionThe aqueous layer was further extracted with ethyl acetate
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe insoluble matter was separated by filtration
  7. customthe solvent was evaporated away
  8. customthe resulting residue was purified by middle-pressure liquid chromatography (eluent, chloroform:methanol=98:2)

出典と根拠

ORDレコード
ord-64761abc99b847f49d8543de2f6a3e16
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07737166B2

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