Water → HCID 86602730、化合物

HRID 1244821ノート

反応式

HRID 1244821 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 10–18° 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-010885194af44b95979420a08d126978
出典データセット
uspto-grants-2006_10
特許番号
US07122672B2

反応ノート

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