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

Methyl 3-bromonaphthalene-1-carboxylate → (3-Bromonaphthalen-1-yl)methanol

HRID 1010621
ノート
印刷プレビュー

反応式

HRID 1010621 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:12](OC)=[O:13])[C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.[H-].C([Al+]CC(C)C)C(C)C>O1CCCC1.C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([CH2:12][OH:13])[C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=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

5

反応物 2

HCID 11311609Methyl 3-bromonaphthalene-1-carboxylateHCID 21225700Diisobutylaluminumhydride

生成物 1

HCID 12749165(3-Bromonaphthalen-1-yl)methanol

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a solution of 5.10 g (19.2 mmol) of the above methyl 3-bromo-1-naphthoate in 20 mL of anhydrous tetrahydrofuran at −78° C. under an atmosphere of nitrogen was added 48 mL (48 mmol) of a 1.0 M solution of diisobutylaluminum hydride in toluene. The resulting solution was allowed to gradually warm to 0° C. over 90 min and quenched with a saturated aqueous solution of potassium sodium tartrate (25 mL). The resulting suspension was vigorously stirred with gradual warming to ambient temperature over 2 h and the layers separated. The aqueous layer was extracted with ethyl acetate (3×20 mL) and the combined organic layers were washed with brine (30 mL), dried over magnesium sulfate, filtered and concentrated in vacuo to afford the title compound as a white solid which was used without further purification LC/MS 237.0 (M+1) and 239.0 (M+3).

後処理

  1. customquenched with a saturated aqueous solution of potassium sodium tartrate (25 mL)
  2. temperaturewith gradual warming to ambient temperature over 2 h
  3. customthe layers separated
  4. extractionThe aqueous layer was extracted with ethyl acetate (3×20 mL)
  5. washthe combined organic layers were washed with brine (30 mL)
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-a91c0f2a82e74b5e8cfdfac903843dd1
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977339B2

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