Phosgene → HCID 22125063、化合物

HRID 1858191ノート

反応式

HRID 1858191 の反応式
[C:1]([NH:5][CH2:6][C:7]1[C:8]([NH:15][CH3:16])=[N:9][C:10]([S:13][CH3:14])=[N:11][CH:12]=1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:24](Cl)(Cl)=[O:25].[Cl-].[NH4+]>O1CCCC1>[C:1]([N:5]1[CH2:6][C:7]2[C:8](=[N:9][C:10]([S:13][CH3:14])=[N:11][CH:12]=2)[N:15]([CH3:16])[C:24]1=[O:25])([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 6371PhosgeneHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 22125127HCID 22125127、化合物

生成物 1

HCID 22125063HCID 22125063、化合物収率 83%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

A mixture of 240 mg (1 mmol) of 5-tert.butylaminomethyl-4-methylamino-2-methylthiopyrimidine and 0.28 ml of triethylamine in 5 ml of tetrahydrofuran was added dropwise to an ice-cooled solution of 1 ml (1.92 mmol) of phosgene (20% solution in toluene) in 5 ml of tetrahydrofuran. After 1 hour 30 ml of saturated aqueous ammonium chloride and 20 ml of tetrahydrofuran were added to the resulting mixture. The phases were separated. The organic phase was dried over magnesium sulfate, filtered and then evaporated to give 220 mg (83%) of 3-tert.butyl-7-methylthio-3,4-dihydro-1-methylpyrimido[4,5-d]pyrimidin-2(1H)-one as a white solid.

後処理

  1. customThe phases were separated
  2. dry with materialThe organic phase was dried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-f19d01b856634e6284350401e22e247d
出典データセット
uspto-grants-2000_11
特許番号
US06150373

反応ノート

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