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Methanesulfonic Acid → 4-Hydroxymethyl-2-meth yl-8-[2'-(1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one

HRID 129015
ノート
印刷プレビュー

反応式

HRID 129015 の反応式
[OH:1][CH2:2][C:3]1[C:4]2[CH2:13][CH2:12][C:11](=[O:14])[N:10]([CH2:15][C:16]3[CH:21]=[CH:20][C:19]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=4[C:28]4[N:32](C(C)(C)C)[N:31]=[N:30][N:29]=4)=[CH:18][CH:17]=3)[C:5]=2[N:6]=[C:7]([CH3:9])[N:8]=1.CS(O)(=O)=O>C1(C)C=CC=CC=1>[OH:1][CH2:2][C:3]1[C:4]2[CH2:13][CH2:12][C:11](=[O:14])[N:10]([CH2:15][C:16]3[CH:17]=[CH:18][C:19]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=4[C:28]4[NH:32][N:31]=[N:30][N:29]=4)=[CH:20][CH:21]=3)[C:5]=2[N:6]=[C:7]([CH3:9])[N:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 193730024-hydroxymethyl-2-methyl-8-[2'-(1-tert-butyl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one

生成物 1

HCID 1784329704-Hydroxymethyl-2-meth yl-8-[2'-(1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one収率 19.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 4-hydroxymethyl-2-methyl-8-[2'-(1-tert-butyl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one (550 mg, 1.14 mmol), methanesulfonic acid (1.10 g, 11.40 mmol), and toluene (10 mL) was heated under reflux for 4 days. The mixture was concentrated, 1N KOH (11.4 mL) was added, and the mixture was extracted with CHCl3 (discarded). The aqueous phase was acidified to pH4-5 with 1N HCl and extracted with CHCl3. The extracts were dried and concentrated to give 94 mg of a yellow foam. Trituration with acetone and recrystallization from EtOH gave 46 mg (9%) of product as a white solid, mp 246°-247° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 days
  3. concentrationThe mixture was concentrated
  4. addition1N KOH (11.4 mL) was added
  5. extractionthe mixture was extracted with CHCl3 (discarded)
  6. extractionextracted with CHCl3
  7. customThe extracts were dried
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-85207125f9f84de9a5ff1d4f7615041e
出典データセット
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05466692

反応ノート

読み込み中…

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