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Diethyl Ether → 6,7-Bis(3-hydroxyphenyl)-pteridin-4-ylamine methanesulfonate salt

HRID 1272468
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HRID 1272468 반응식
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[OH:6][C:7]1[CH:8]=[C:9]([C:13]2[N:14]=[C:15]3[C:20](=[N:21][C:22]=2[C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([OH:29])[CH:24]=2)[N:19]=[CH:18][N:17]=[C:16]3[NH2:30])[CH:10]=[CH:11][CH:12]=1.C(OCC)C>CO>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[OH:6][C:7]1[CH:8]=[C:9]([C:13]2[N:14]=[C:15]3[C:20](=[N:21][C:22]=2[C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([OH:29])[CH:24]=2)[N:19]=[CH:18][N:17]=[C:16]3[NH2:30])[CH:10]=[CH:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 6395Methanesulfonic AcidHCID 100880663-[4-Amino-7-(3-hydroxyphenyl)pteridin-6-yl]phenol

생성물 1

HCID 865941386,7-Bis(3-hydroxyphenyl)-pteridin-4-ylamine methanesulfonate salt수율 97.11%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

1.308 g (13.63 mmol) of methanesulfonic acid in 10 mL of MeOH was added to the suspension of 2.15 g (6.48 mmol) of 6,7-bis(3-hydroxyphenyl)-pteridin-4-ylamine in 10 mL of MeOH. The mixture became homogeneous and orange-red in color. It was stirred for 30 min and then added dropwise to 400 mL of diethyl ether with vigorous stirring. The formed yellow precipitate was collected, washed with diethyl ether and dried in vacuo to give 2.69 g (97.11% yield) of the product as a light-yellow powder. Mass-spec [ES+]=332.8. 1H NMR (MeOH-d4) 2.70 (3H, s), 6.86–6.90 (2H, m), 6.99–7.01 (2H, m), 7.04–7.08 (2H, m), 7.16–7.21 (2H, m), 8.80 (1H, s).

후처리

  1. customThe formed yellow precipitate was collected
  2. washwashed with diethyl ether
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-00ca0ef48ae6460abf535c4db1d89927
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07208493B2

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