Water → HCID 86602730、化合物

HRID 2222304ノート

反応式

HRID 2222304 の反応式
Cl.[Cl:2][CH2:3][CH2:4][CH2:5][C:6]#[C:7][C:8]([NH2:11])([CH3:10])[CH3:9].C(N(CC)CC)C.[Br:19][CH:20]([CH2:24][CH3:25])[C:21](Br)=[O:22].O>ClCCl>[Br:19][CH:20]([CH2:24][CH3:25])[C:21]([NH:11][C:8]([CH3:10])([CH3:9])[C:7]#[C:6][CH2:5][CH2:4][CH2:3][Cl:2])=[O:22]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 1172932-Bromobutanoyl bromideHCID 86602731HCID 86602731、化合物

生成物 1

HCID 86602730HCID 86602730、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
5 °C

実験手順

The product from Step 2 (12.2 g) was suspended in dry dichloromethane (300 ml), cooled to 5° C. with stirring and dry triethylamine (18.1 ml) was added. The mixture was stirred for 0.25 hours and 2-bromobutyryl bromide (14.3 g) in dichloromethane (25 ml) was added dropwise over 0.5 hours at 10-8° C. The mixture was stirred for a further 0.5 hours then allowed to warm to ambient temperature for 2 hours and stored for 18 hours. Water was added and the organic phase was separated, washed with water (three times), dried over magnesium sulphate then evaporated under reduced pressure to give the required product as a dark yellow oil, 17.4 g, 1H NMR (CDCl3) δ: 1.04(3H, t); 1.62(6H, s); 1.96(2H, m); 2.10(2H, m); 2.38(2H, m); 3.66(2H, t); 4.12(1H, t); 6.44(1H, s).

後処理

  1. stirringThe mixture was stirred for 0.25 hours
  2. stirringThe mixture was stirred for a further 0.5 hours
  3. temperatureto warm to ambient temperature for 2 hours
  4. customthe organic phase was separated
  5. washwashed with water (three times)
  6. dry with materialdried over magnesium sulphate
  7. customthen evaporated under reduced pressure

出典と根拠

ORDレコード
ord-ff0113344d6f44cf80c9a32cc4e8c65c
出典データセット
uspto-grants-2008_05
特許番号
US07371764B2

反応ノート

読み込み中…