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Glycidyl methacrylate → 3-Ethoxy-4-hydroxymandelic acid

HRID 2165712
ノート
印刷プレビュー

反応式

HRID 2165712 の反応式
C[Si](C)(C)O[C:4]([O:8]C)=[C:5]([CH3:7])[CH3:6].ClC1C=C(C=CC=1)[C:16]([O-:18])=[O:17].C([N+](CCCC)(CCCC)CCCC)CCC.[C:39]([O:44][CH2:45][CH:46]1[O:48][CH2:47]1)(=O)[C:40](C)=C.C(OCC(CC)CCCC)(=O)C(C)=C>C(#N)C.CO.O1CCCC1.C1(C)C(C)=CC=CC=1.O1CCCC1.C1COCC1>[CH3:40][CH2:39][O:44][C:45]1[CH:6]=[C:5]([CH:4]([OH:8])[C:16]([OH:18])=[O:17])[CH:7]=[CH:47][C:46]=1[OH:48]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 4

HCID 7837Glycidyl methacrylate2 回HCID 127132-Ethylhexyl methacrylateHCID 552336Silane, ((1-methoxy-2-methyl-1-propenyl)oxy)trimethyl-HCID 21922187Tetrabutylammonium m-chlorobenzoate2 回

生成物 1

HCID 1937923-Ethoxy-4-hydroxymandelic acid

試薬・触媒・溶媒 5

HCID 887
Methanol
溶媒
3 回
HCID 6342Acetonitrile溶媒
HCID 7237O-Xylene溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 22180045THF tetrahydrofurane溶媒

反応条件

温度
10 °C

実験手順

A 250 ml round bottom flask, equipped with a mechanical stirrer, thermometer, and nitrogen inlet, is charged with tetrahydrofuran THF (75.6 gm), 1-trimethylsiloxy-1-methoxy-2-methylpropene (7.0 gm, 0.0402M), xylene (1.0 gm), and tetrabutylammonium m-chlorobenzoate (400 μl of a 1.0M solution in acetonitrile). The flask is cooled to 10° C. Feed I consists of tetrahydrofuran (4.0 gm) and tetrabutylammonium m-chlorobenzoate (400 μl of a 1.0M solution). It is added over 50 minutes. Feed II is glycidyl methacrylate (17.3 gm, 0.122M). It is started simultaneously with the start of the feed I. Feed II is added over one minute. Feed III is 2-ethylhexyl methacrylate (40.7 gm, 0.206M). Feed III is started 9 minutes after feed I has begun. Feed III is added over 30 minutes. The temperature of the flask rises to about 41.0° C. After feed I is completed the flask is cooled to 10° C. Feed IV is glycidyl methacrylate (17.1 gm, 0.120M). It is started 8 minutes after feed I is completed. Feed IV is added over 1 minute. At 70 minutes of total reaction time (11 minutes after feed IV is completed) methanol (10.0 gm) is added to the flask.

後処理

  1. customA 250 ml round bottom flask, equipped with a mechanical stirrer
  2. additionIt is added over 50 minutes
  3. customrises to about 41.0° C
  4. temperatureis cooled to 10° C

出典と根拠

ORDレコード
ord-a4a00c4dab1444919ec22db641660e9d
出典データセット
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04940761

反応ノート

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