p-Toluenesulfonic acid monohydrate → HCID 178485563、化合物

HRID 334149ノート

反応式

HRID 334149 の反応式
[CH3:1][NH:2][C:3]([C:5]1[N:6](C2CCCCO2)[C:7]2[C:12]([N:13]=1)=[C:11]([N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)[N:10]=[C:9]([Cl:20])[N:8]=2)=[O:4].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO.O.C(=O)(O)[O-].[Na+]>[CH3:1][NH:2][C:3]([C:5]1[NH:6][C:7]2[C:12]([N:13]=1)=[C:11]([N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)[N:10]=[C:9]([Cl:20])[N:8]=2)=[O:4]

参加物

6

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 86667366HCID 86667366、化合物

生成物 1

HCID 178485563HCID 178485563、化合物収率 70%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

2-Chloro-6-morpholin-4-yl-9-(tetrahydro-pyran-2-yl)-9H-purine-8-carboxylic acid methylamide (104 mg, 0.27 mmol) was suspended in methanol (6 mL) and p-toluenesulfonic acid monohydrate (10 mg, 0.05 mmol) was added. The mixture was stirred at room temperature for 68 h, then diluted with water and neutralized with aqueous sodium bicarbonate. The solid precipitate was filtered off and dried at 50° C. under vacuum to give 2-chloro-6-morpholin-4-yl-9H-purine-8-carboxylic acid methylamide (56 mg, 70%). LCMS RT=2.43, [M+H]+=297/299

後処理

  1. filtrationThe solid precipitate was filtered off
  2. customdried at 50° C. under vacuum

出典と根拠

ORDレコード
ord-1492cf5858164a5db651a26bd2467990
出典データセット
uspto-grants-2014_11
特許番号
US08883799B2

反応ノート

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