Carbon tetrabromide → HCID 20062834、化合物

HRID 2166155ノート

反応式

HRID 2166155 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:20]1([CH2:26][CH2:27][O:28][CH2:29][C:30]#[C:31][CH2:32][CH2:33]O)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(Br)(Br)(Br)[Br:36]>C(Cl)Cl>[Br:36][CH2:33][CH2:32][C:31]#[C:30][CH2:29][O:28][CH2:27][CH2:26][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

参加物

5

反応物 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 20062817HCID 20062817、化合物

生成物 1

HCID 20062834HCID 20062834、化合物収率 52.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of triphenylphosphine (5.25 g) in dry DCM (15 ml) was added to a solution of the product of step (ii) (3.9 g) and carbon tetrabromide (6.63 g) in dry DCM (25 ml) at 0° over 10 min. The yellow solution was stirred at 0° for 30 min, evaporated onto silica (Merck 9385) and purified by FCC eluting with H→H-ER (3:1) to give the title compound as a colourless oil (2.7 g). T.l.c. (H-ER 2:1) Rf 0.69.

後処理

  1. customevaporated onto silica (Merck 9385)
  2. custompurified by FCC
  3. washeluting with H→H-ER (3:1)

出典と根拠

ORDレコード
ord-006d27edad214f0dbc2169b910944382
出典データセット
uspto-grants-1990_07
特許番号
US04943591

反応ノート

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