Phosgene → HCID 22125063, 화합물

HRID 1858191노트

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HRID 1858191 반응식
[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]

참가 물질

6

반응물 4

HCID 6371PhosgeneHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 22125127HCID 22125127, 화합물

생성물 1

HCID 22125063HCID 22125063, 화합물수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f19d01b856634e6284350401e22e247d
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06150373

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