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Water → Methyl 3-(2-cyanopyrrol-1-yl)benzoate

HRID 399863
ノート
印刷プレビュー

反応式

HRID 399863 の反応式
ClS([N:5]=[C:6]=O)(=O)=O.[N:8]1([C:13]2[CH:14]=[C:15]([CH:20]=[CH:21][CH:22]=2)[C:16]([O:18][CH3:19])=[O:17])[CH:12]=[CH:11][CH:10]=[CH:9]1.CN(C)C=O.O>ClCCl>[C:6]([C:12]1[N:8]([C:13]2[CH:14]=[C:15]([CH:20]=[CH:21][CH:22]=2)[C:16]([O:18][CH3:19])=[O:17])[CH:9]=[CH:10][CH:11]=1)#[N:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 70918Chlorosulfonyl isocyanateHCID 3322314Methyl 3-(1H-pyrrol-1-yl)benzoate

生成物 1

HCID 18945318Methyl 3-(2-cyanopyrrol-1-yl)benzoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Chlorosulfonyl isocyanate (18.2 ml) was dropwise added to a solution of methyl 3-(pyrrol-1-yl)benzoate (35.0 g) in dichloromethane (350 ml) at -10°~20° C. and the mixture was stirred for 1 hour at the same temperature. To the mixture was dropwise added N,N-dimethylformamide (105 ml) at the same temperature and the mixture was stirred for 1 hour at 0°-5° C. The reaction mixture was poured into water. The separated organic layer was washed with saturated aqueous sodium bicarbonate solution and water. The organic solution was dried over magnesium sulfate and evaporated in vacuo to give methyl 3-(2-cyanopyrrol-1-yl)benzoate (30.67 g).

後処理

  1. stirringthe mixture was stirred for 1 hour at 0°-5° C
  2. washThe separated organic layer was washed with saturated aqueous sodium bicarbonate solution and water
  3. dry with materialThe organic solution was dried over magnesium sulfate
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-9a1d0727ce7e4f48b6f76e523f48377d
出典データセット
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05824691

反応ノート

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