Naphthalene → n-Butyl 2-hydroxy-3-butenoate

HRID 1099475

反応式

HRID 1099475 の反応式
C(O)[C@H]1[O:7][C@H:6]([O:8][C@:9]2(CO)O[C@H:12](CO)[C@@H:11](O)[C@@H:10]2O)[C@H:5]([OH:20])[C@@H:4](O)[C@@H:3]1O.C1C2C(=CC=CC=2)C=CC=1.C(OCCCC)(=O)C(C)O>C(O)CCC>[OH:20][CH:5]([CH:4]=[CH2:3])[C:6]([O:8][CH2:9][CH2:10][CH2:11][CH3:12])=[O:7]

参加物

5

反応物 3

HCID 931NaphthaleneHCID 5988SucroseHCID 8738Butyl Lactate

生成物 1

HCID 86641725n-Butyl 2-hydroxy-3-butenoate収率 25%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
160 °C

実験手順

An autoclave (50 cc microclave) is charged with 8.0 g of 1-butanol, 0.2249 g of sucrose (0.6569 mmol), 121.0 mg naphthalene (internal standard) and finally with 160.5 mg Sn-BEA (prepared according to U.S. Pat. No. 6,306,364). The autoclave is closed, charged with 20 bar of argon and heated to 160° C. After the temperature reaches 100° C., the mechanical stirrer is started (500 rpm) and the mixture is heated for 20 hours under these conditions. GC-analysis of the reaction mixture shows that 0.68 mmol of n-butyl lactate is formed (26%) together with 0.164 mmol n-butyl 2-hydroxy-3-butenoate (8%).

後処理

  1. customprepared
  2. customThe autoclave is closed
  3. additioncharged with 20 bar of argon
  4. customreaches 100° C.
  5. temperaturethe mixture is heated for 20 hours under these conditions

出典と根拠

ORDレコード
ord-544737580ae24e6e90d0d48571473755
出典データセット
uspto-grants-2012_03
特許番号
US08143439B2

関連ノート

読み込み中…