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4-Amino-6-chlorotoluene-2-sulphonic acid → O-{[(3-chloro-4-methyl-5-sulfophenyl)amino]carbonyl}-L-serine

HRID 330867
ノート
印刷プレビュー

反応式

HRID 330867 の反応式
[NH:1](C(OC(C)(C)C)=O)[C@H:2]([C:5]([O:7]C(C)(C)C)=[O:6])CO.[NH2:19][C:20]1[CH:21]=[C:22]([Cl:31])[C:23]([CH3:30])=[C:24]([S:26]([OH:29])(=[O:28])=[O:27])[CH:25]=1.ClC(Cl)(O[C:36](=[O:42])[O:37][C:38](Cl)(Cl)Cl)Cl.CCN(C(C)C)C(C)C>C(Cl)Cl>[Cl:31][C:22]1[CH:21]=[C:20]([NH:19][C:36]([O:37][CH2:38][C@@H:2]([C:5]([OH:7])=[O:6])[NH2:1])=[O:42])[CH:25]=[C:24]([S:26]([OH:29])(=[O:27])=[O:28])[C:23]=1[CH3:30]
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 808054-Amino-6-chlorotoluene-2-sulphonic acidHCID 81531DiisopropylethylamineHCID 94429TriphosgeneHCID 7019054Boc-Ser-Otbu

生成物 1

HCID 45275789O-{[(3-chloro-4-methyl-5-sulfophenyl)amino]carbonyl}-L-serine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

Boc-Ser-OtBu, 100 mg (0.38 mmol), 86 mg (0.38 mmol) of 5-amino-3-chloro-2-methylbenzenesulfonic acid and 37 mg (0.0127 mmol) of triphosgene were suspended in 1 ml of methylene chloride, and 66 μl (0.76 mmol) of DIEA was added to the suspension. After stirring at room temperature overnight, the solvent was removed by distillation. The mixture was purified according to the purification step A to give the protected title compound. The protected product obtained was dissolved in 2 ml of trifluoroacetic acid and stirred for 2 hours. The solvent was then removed by distillation and the mixture was purified according to the purification step A to give the title compound.

後処理

  1. customthe solvent was removed by distillation
  2. customThe mixture was purified
  3. customaccording to the purification step A

出典と根拠

ORDレコード
ord-715ab3645524440fab104abf76bc6b00
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877739B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート