Thionyl Chloride → 10-Methylacridan-9-carboxylic acid chloride

HRID 1034584ノート

反応式

HRID 1034584 の反応式
[CH3:1][N:2]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:9]([C:16]([OH:18])=O)[C:8]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]1=2.S(Cl)([Cl:21])=O.C1C(N=NC2C=CC(N)=C(S([O-])(=O)=O)C=2)=CC=C(S([O-])(=O)=O)C=1.[Na+].[Na+]>ClCCl>[CH3:1][N:2]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:9]([C:16]([Cl:21])=[O:18])[C:8]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]1=2

参加物

5

反応物 3

HCID 24386Thionyl ChlorideHCID 75918Benzenesulfonic acid, 2-amino-5-(2-(4-sulfophenyl)diazenyl)-, sodium salt (1:?)HCID 1039934110-Methylacridan-9-carboxylic acid

生成物 1

HCID 5452072910-Methylacridan-9-carboxylic acid chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Into a 50 mL round bottom flask equipped with magnetic stirrer and under an argon atmosphere was charged a solution of 0.305 parts of 10-methylacridan-9-carboxylic acid (77) in 15 mL of dichloromethane and cooled to 5° C. (ice-water). Then, 1.05 parts of thionyl chloride was added to the cold yellow acid solution and stirred for 1.5 hr at a temperature below 15° C. The light red brown solution was concentrated under reduced pressure and the residue was dried for 15 min to give acid chloride (78).

後処理

  1. customInto a 50 mL round bottom flask equipped with magnetic stirrer and under an argon atmosphere
  2. concentrationThe light red brown solution was concentrated under reduced pressure
  3. customthe residue was dried for 15 min

出典と根拠

ORDレコード
ord-7aa3577afe0645c797e04fc91e72a4c2
出典データセット
uspto-grants-2013_10
特許番号
US08546150B2

反応ノート

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