Hydrochloric Acid → HCID 19380609、化合物

HRID 466495ノート

反応式

HRID 466495 の反応式
C([Li])CCC.[F:6][C:7]1[CH:8]=[C:9]([CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH:10]=[C:11]([F:13])[CH:12]=1.[B:19](OC(C)C)([O:24]C(C)C)[O:20]C(C)C.Cl>C1COCC1>[F:6][C:7]1[CH:8]=[C:9]([CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH:10]=[C:11]([F:13])[C:12]=1[B:19]([OH:24])[OH:20]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 21531Triisopropyl borateHCID 157519781,3-Difluoro-5-pentylbenzeneHCID 178418339Butyllithium

生成物 1

HCID 19380609HCID 19380609、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of n-butyllithium (10.4M in hexane; 2.70 ml, 0.028 mol) was added dropwise to a stirred, cooled (-78° C.) solution of compound 13 (5.00 g, 0.027 mol) in dry THF (60 ml) under dry nitrogen. The stirred mixture was maintained under these conditions for 2.5 h and a previously cooled solution of tri-isopropyl borate (10.22 g, 0.054 mol) in dry THF (50 ml) was added dropwise at -78° C. The stirred mixture was allowed to warm to room temperature overnight and stirred for 1 h with 10% hydrochloric acid (30 ml). The product was extracted into ether (twice), and the combined ethereal extracts were washed with water and dried (MgSO4). The solvent was removed in vacuo to give a colourless solid.

後処理

  1. temperatureThe stirred mixture was maintained under these conditions for 2.5 h
  2. extractionThe product was extracted into ether (twice), and the combined ethereal extracts
  3. washwere washed with water
  4. dry with materialdried (MgSO4)
  5. customThe solvent was removed in vacuo
  6. customto give a colourless solid

出典と根拠

ORDレコード
ord-6154afb57e054b5183ec35d6077b2941
出典データセット
uspto-grants-1992_10
特許番号
US05156763

反応ノート

読み込み中…