4-Methylmorpholine → 2-(2-Nitrophenyl)propyl chloroformate

HRID 354210ノート

反応式

HRID 354210 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH:10]([CH3:13])[CH2:11][OH:12])([O-:3])=[O:2].CN1CCOCC1.O=C(Cl)[O:23][C:24](Cl)(Cl)[Cl:25]>C1COCC1>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH:10]([CH3:13])[CH2:11][O:12][C:24]([Cl:25])=[O:23])([O-:3])=[O:2]

参加物

5

反応物 3

HCID 79724-MethylmorpholineHCID 10426DiphosgeneHCID 113897552-(2-Nitrophenyl)propan-1-ol

生成物 1

HCID 114479052-(2-Nitrophenyl)propyl chloroformate収率 71.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

A solution consisting of 7.2 g 2-(2-nitrophenyl)propanol (39.7 mmol) and 4.4 ml N-methylmorpholine (39.7 mmol) in 15 ml absolute THF are slowly added to 5 ml diphosgene (41.4 mmol) in 10 ml absolute THF at 0° C. in a nitrogen atmosphere through a needle. Having stirred for 1 hour at 0° C., some of the precipitate is sucked off and the filtrate is withdrawn at the high vacuum. 6.91 g of (1) is obtained in the form of a brown oil (71%).

後処理

  1. customthe filtrate is withdrawn at the high vacuum

出典と根拠

ORDレコード
ord-995f6925fda549a19df6a335d826d746
出典データセット
uspto-grants-2004_06
特許番号
US06756492B1

反応ノート

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