Glyoxylic Acid → 37662-06-9

HRID 2305252ノート

反応式

HRID 2305252 の反応式
[CH3:1][C@H:2]([NH2:9])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:10]1([CH3:16])C=CC=CC=1.[C:17]([OH:21])(=[O:20])[CH:18]=O>O>[C:3]1([C@@H:2]([N:9]=[CH:18][C:17]([O:21][CH2:10][CH3:16])=[O:20])[CH3:1])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 760Glyoxylic Acid2 回HCID 1140TolueneHCID 758181-Phenethylamine, (-)-

生成物 1

HCID 1146979737662-06-9

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
-5 °C

実験手順

The synthesis was performed according to the procedure reported in the literature. (S)-(−)-α-Methylbenzylamine (238.6 g, 1.964 mol) was added into 2 L round bottom flask equipped a stirrer bar. Toluene (520 mL) was added. The reaction mixture was cooled to −5° C., and was allowed to stir for 10 min. Glyoxylic acid (200 g, 1.96 mol) was tranferred to a dropping funnel and was added slowly to the cooled reaction mixture for approximately 15 min. As the addition of the glyoxylic acid proceeded, the reaction mixture became cloudy and the flask became warm. The mixture was allowed to stir for 10 min after the addition. When the reaction was complete, the water generated during the reaction was removed. The organic layer was dried over Na2SO4, filtered via Buchner funnel, rinsed with toluene, concentrated in vacuo to yield an oil which was used directly in the next step.

後処理

  1. customequipped a stirrer bar
  2. additionwas added slowly to the cooled reaction mixture for approximately 15 min
  3. temperaturethe flask became warm
  4. stirringto stir for 10 min
  5. additionafter the addition
  6. customwas removed
  7. dry with materialThe organic layer was dried over Na2SO4
  8. filtrationfiltered via Buchner funnel
  9. washrinsed with toluene
  10. concentrationconcentrated in vacuo
  11. customto yield an oil which

出典と根拠

ORDレコード
ord-a00c6d6ac8a34941bfd8680d20d7c68b
出典データセット
uspto-grants-2002_08
特許番号
US06440417B1

反応ノート

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