Azido(trimethyl)stannane → HCID 178451517, 화합물

HRID 602962노트

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HRID 602962 반응식
[C:1]([C:3]1[N:4]=[CH:5][C:6]2[CH2:11][N:10]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:9][C:7]=2[N:8]=1)#[N:2].[N:19]([Sn](C)(C)C)=[N+:20]=[N-:21]>C1(C)C=CC=CC=1>[NH:19]1[C:1]([C:3]2[N:4]=[CH:5][C:6]3[CH2:11][N:10]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:9][C:7]=3[N:8]=2)=[N:2][N:21]=[N:20]1

참가 물질

4

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HCID 5104973Azido(trimethyl)stannaneHCID 184428191,1-Dimethylethyl 2-cyano-5,7-dihydro-6H-pyrrolo[3,4-d]pyrimidine-6-carboxylate2회

생성물 1

HCID 178451517HCID 178451517, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
110 °C

실험 절차

To a solution of tert-butyl 2-cyano-5,7-dihydro-6H-pyrrolo[3,4-d]pyrimidine-6-carboxylate (Intermediate 9, Step D) (71 mg, 0.29 mmol) in toluene was added azidotrimethyltin (596 mg, 2.9 mmol). The resulting mixture was heated at 110° C. overnight. After the solvent was removed under reduced pressure, the residue was purified by reverse-phase silica gel chromatography (gradient 5-50% acetonitrile in water containing 0.1% TFA) to yield tert-butyl 2-(1H-tetrazol-5-yl)-5,7-dihydro-6H-pyrrolo[3,4-d]pyrimidine-6-carboxylate. The product was treated as described for Intermediate 9, Step E, to yield the title compound.

후처리

  1. customAfter the solvent was removed under reduced pressure
  2. customthe residue was purified by reverse-phase silica gel chromatography (gradient 5-50% acetonitrile in water containing 0.1% TFA)

출처 및 근거

ORD 기록
ord-a2e4521f41304a8682bb751db6663fbc
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906649B2

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