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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Diglyme → HCID 178527889, 화합물

HRID 387769
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HRID 387769 반응식
P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:2].C(=O)(O)[O-].[Na+].COCCOCCOC.[C:29]1([C:35]2[NH:44][C:38]3[N:39]=[CH:40][N:41]=[C:42](O)[C:37]=3[CH:36]=2)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>O>[C:29]1([C:35]2[NH:44][C:38]3[N:39]=[CH:40][N:41]=[C:42]([SH:2])[C:37]=3[CH:36]=2)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8150DiglymeHCID 14817Phosphorus sulfide (P2S5)3회HCID 516892Sodium Bicarbonate3회HCID 178518053HCID 178518053, 화합물

생성물 1

HCID 178527889HCID 178527889, 화합물수율 94.8%

시약·촉매·용매 1

HCID 962Water
용매

실험 절차

After adding 6.19 g of phosphorus pentasulfide, 6.24 g of sodium bicarbonate and 25 ml of diglyme to 2.45 g of the 6-phenyl-7H-pyrrolo[2,3-d]pyrimidin-4-ol described in WO97/02266 and PCT/EP96/02728, and stirring the mixture for 1 hour, an additional 3 g of phosphorus pentasulfide and 3 g of sodium bicarbonate were added and the mixture was stirred for 1 hour. There were further added another 3 g of phosphorus pentasulfide and 3 g of sodium bicarbonate, and the mixture was stirred for 1 hour. It was then returned to room temperature, water was added, the mixture was stirred for 10 minutes, and the precipitated crystals were filtered out, washed with water and dried to obtain 2.5 g of the title compound.

후처리

  1. stirringthe mixture was stirred for 1 hour
  2. stirringthe mixture was stirred for 1 hour
  3. customwas then returned to room temperature
  4. stirringthe mixture was stirred for 10 minutes
  5. filtrationthe precipitated crystals were filtered out
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-d0c4a62584cb46a88859215a7bb7b6cb
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372981B2

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