Formaldehyde → 3-acetyl-N,N-dibenzyl-3-aminomethyltetrahydrofuran-2-one

HRID 2300999ノート

反応式

HRID 2300999 の反応式
[CH2:1]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16]=O.[C:18]([CH:21]1[CH2:25][CH2:24][O:23][C:22]1=[O:26])(=[O:20])[CH3:19]>O>[C:18]([C:21]1([CH2:16][N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:25][CH2:24][O:23][C:22]1=[O:26])(=[O:20])[CH3:19]

参加物

5

反応物 3

HCID 712FormaldehydeHCID 7656DibenzylamineHCID 106012-Acetylbutyrolactone

生成物 1

HCID 102687063-acetyl-N,N-dibenzyl-3-aminomethyltetrahydrofuran-2-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

To a mixture of 10.2 g of dibenzylamine and 29.7 g of water, 8.9 g of 37% by weight formaldehyde aqueous solution was added dropwise at room temperature, followed by dropwise addition of 12.8 g of 3-acetyltetrahydrofuran-2-one at room temperature. After the completion of addition, the mixture was heated to 90° C. and thereby yielded a solution. The solution was cooled to room temperature, was filtrated, the resulting solid matter was heated with diethyl ether and thereby yielded a solution. The solution was gradually cooled to 0° C., the resulting crystal was filtrated and thereby yielded 19.2 g of 3-acetyl-N,N-dibenzyl-3-aminomethyltetrahydrofuran-2-one as a white crystal.

後処理

  1. additionwas added dropwise at room temperature
  2. additionAfter the completion of addition
  3. customyielded a solution
  4. temperatureThe solution was cooled to room temperature
  5. filtrationwas filtrated
  6. temperaturethe resulting solid matter was heated with diethyl ether
  7. customyielded a solution
  8. temperatureThe solution was gradually cooled to 0° C.
  9. filtrationthe resulting crystal was filtrated

出典と根拠

ORDレコード
ord-9f6a9870189243b7bebd41854e0b7a97
出典データセット
uspto-grants-2002_12
特許番号
US06498258B2

反応ノート

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