4-Methylmorpholine → HCID 71623011、化合物

HRID 1477510ノート

反応式

HRID 1477510 の反応式
[NH2:1][C:2]([CH3:6])([CH3:5])[C:3]#[N:4].CN1CC[O:11][CH2:10][CH2:9]1.O1C=[C:17]([C:19](Cl)=[O:20])[N:16]=[N:15]1>ClCCl>[C:3]([C:2]([NH:1][C:19]([C:17]1[O:11][C:10]([CH3:9])=[N:15][N:16]=1)=[O:20])([CH3:6])[CH3:5])#[N:4]

参加物

5

反応物 3

HCID 79724-MethylmorpholineHCID 880222-Amino-2-methylpropionitrileHCID 89656276HCID 89656276、化合物

生成物 1

HCID 71623011HCID 71623011、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

2-Amino-2-methylpropanenitrile (90 gms) was suspended in dichloromethane (90 ml) and N-methyl morpholine (1.10 moles) was added with stirring. A mixture of oxadiazole carbonyl chloride (90 gms) in dichloromethane (100 ml) was added drop wise to the suspension at 0 to 5° C. The reaction mixture was stirred and monitored by thin layer chromatography (TLC). The reaction mass was concentrated under reduced pressure after completion of reaction. The product separated out on addition of isopropyl alcohol (500 ml), which was then filtered and dried.

後処理

  1. additionwas added drop wise to the suspension at 0 to 5° C
  2. stirringThe reaction mixture was stirred
  3. concentrationThe reaction mass was concentrated under reduced pressure
  4. customafter completion of reaction
  5. customThe product separated out on addition of isopropyl alcohol (500 ml), which
  6. filtrationwas then filtered
  7. customdried

出典と根拠

ORDレコード
ord-0732dca887ce45029ae35522cc088920
出典データセット
uspto-grants-2016_08
特許番号
US09403809B2

反応ノート

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