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

Water → 2-(2-tert-Butyl-1H-tetrazol-5-yl)phenyltri-n-butylstannane

HRID 1440463
ノート
印刷プレビュー

反応式

HRID 1440463 の反応式
C([N:5]1[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2Br)=[N:8][N:7]=[N:6]1)(C)(C)C.[Li]C[CH2:19][CH2:20][CH3:21].[CH2:22]([Sn:26](Cl)([CH2:31][CH2:32][CH2:33][CH3:34])[CH2:27][CH2:28][CH2:29][CH3:30])[CH2:23][CH2:24][CH3:25].O.[CH2:37]1COCC1>>[C:20]([N:7]1[NH:6][N:5]=[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[Sn:26]([CH2:31][CH2:32][CH2:33][CH3:34])([CH2:27][CH2:28][CH2:29][CH3:30])[CH2:22][CH2:23][CH2:24][CH3:25])[NH:8]1)([CH3:19])([CH3:21])[CH3:37]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 962WaterHCID 8028TetrahydrofuranHCID 15096Tributyltin Chloride2 回HCID 218408841-tert-Butyl-5-(2-bromophenyl)-1H-tetrazoleHCID 178418339Butyllithium

生成物 1

HCID 676965402-(2-tert-Butyl-1H-tetrazol-5-yl)phenyltri-n-butylstannane収率 45%

実験手順

To a cooled (-78° C.) solution of 1-tert-butyl-5-(2-bromophenyl)-1H-tetrazole (12.3 g, 0.043 mol), prepared as described in Step 3 of the Example 3 alternative synthesis, in THF (80 mL) was added 1.6M nBuLi in hexanes (32.7 mL, 0.052 mol). After 1 h, tri-n-butyltin chloride (17.1 g, 0.052 mol) was added and stirring was continued for 3 h at -78° C. The mixture was warmed to room temperature and stirred for 18 h. Water was added and the mixture was extracted with ether. The combined extracts were washed with water, brine, dried (MgSO4), and concentrated to give a brown oil. Excess tri-n-butyltin chloride and remaining starting material were removed by distillation under high vacuum to give 9.6 g (45%) of product as a brown oil.

後処理

  1. customprepared
  2. waitwas continued for 3 h at -78° C
  3. stirringstirred for 18 h
  4. extractionthe mixture was extracted with ether
  5. washThe combined extracts were washed with water, brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated
  8. customto give a brown oil
  9. customwere removed by distillation under high vacuum

出典と根拠

ORDレコード
ord-8c08ab3b4c0f447e9732c003643ec903
出典データセット
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05498776

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート