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Tetrahydrofuran → HCID 22805384、化合物

HRID 1706628
ノート
印刷プレビュー

反応式

HRID 1706628 の反応式
[CH3:1][C@@:2]1([C:8](O)=[O:9])[CH2:6][CH2:5][C:4](=[O:7])[O:3]1.O1CCCC1>O>[OH:9][CH2:8][C@@:2]1([CH3:1])[O:3][C:4](=[O:7])[CH2:5][CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8028TetrahydrofuranHCID 53249432(2S)-2-Methyl-5-oxooxolane-2-carboxylic acid

生成物 1

HCID 22805384HCID 22805384、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 14.8 g. (102.7 mmol) of (S)-(-)-2-methyl-5-oxotetrahydro-2-furoic acid mp 84°-87° C.; [α]25D-16.56° in 70 ml. of dry tetrahydrofuran (THF) was added 10.1 ml. (8.1 g.; 106.7 mmol) of borane-methyl sulphide complex, dropwise, with stirring over a 0.5 hr. period. Occasional ice-bath cooling was employed to maintain the internal temperature below 30°. After stirring at room temperature for 1.5 hr., the reaction mixture was cautiously decomposed by the dropwise addition of 6.2 ml. of H2O. The mixture was then concentrated under water aspirator pressure and the residue was taken up in ethyl acetate and filtered. The solids were washed thoroughly with ethyl acetate and filtered. The solids were washed thoroughly with ethyl acetate and the filtrate and washes were combined and concentrated in vacuo giving (S)-(+)-5-(hydroxymethyl)-5-methyldihydro-2(3H)-furanone as a colorless oil (13.6 g.) which was used without further purification.

後処理

  1. temperatureOccasional ice-bath cooling
  2. temperatureto maintain the internal temperature below 30°
  3. stirringAfter stirring at room temperature for 1.5 hr
  4. addition, the reaction mixture was cautiously decomposed by the dropwise addition of 6.2 ml
  5. concentrationThe mixture was then concentrated under water aspirator pressure
  6. filtrationfiltered
  7. washThe solids were washed thoroughly with ethyl acetate
  8. filtrationfiltered
  9. washThe solids were washed thoroughly with ethyl acetate
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-80644101c3194e62920df8a677b6291f
出典データセット
uspto-grants-1980_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04208331

反応ノート

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