p-Toluenesulfonic acid monohydrate → HCID 178485563, 화합물

HRID 334149노트

반응식

HRID 334149 반응식
[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]

참가 물질

6

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 86667366HCID 86667366, 화합물

생성물 1

HCID 178485563HCID 178485563, 화합물수율 70%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 516892Sodium Bicarbonate용매

실험 절차

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

후처리

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

출처 및 근거

ORD 기록
ord-1492cf5858164a5db651a26bd2467990
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883799B2

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