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Sodium Methoxide → 2-Methoxy-5,6-dimethyl-8-propyl-3-thia-1,4,7,8a-tetraaza-as-indacene

HRID 1051430
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HRID 1051430 반응식
Br[C:2]1[S:13][C:12]2[N:11]=[C:10]([CH3:14])[C:9]3[N:5]([C:6]([CH2:16][CH2:17][CH3:18])=[N:7][C:8]=3[CH3:15])[C:4]=2[N:3]=1.[CH3:19][O-:20].[Na+]>CO>[CH3:19][O:20][C:2]1[S:13][C:12]2[N:11]=[C:10]([CH3:14])[C:9]3[N:5]([C:6]([CH2:16][CH2:17][CH3:18])=[N:7][C:8]=3[CH3:15])[C:4]=2[N:3]=1
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참가 물질

4

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HCID 10942334Sodium MethoxideHCID 867155612-Bromo-5,6-dimethyl-8-propyl-3-thia-1,4,7,8a-tetraaza-as-indacene

생성물 1

HCID 734259732-Methoxy-5,6-dimethyl-8-propyl-3-thia-1,4,7,8a-tetraaza-as-indacene

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

2-Bromo-5,6-dimethyl-8-propyl-3-thia-1,4,7,8a-tetraaza-as-indacene was dissolved in 5 mL of methanol and sodium methoxide (4.98 mg, 0.092 mmol) was added. The resulting mixture was stirred at 60° C. for 1 h. LC-MS showed complete consumption of 2-bromo-5,6-dimethyl-8-propyl-3-thia-1,4,7,8a-tetraaza-as-indacene. After removal of the solvent under reduced pressure, 5 mL of water and 10 mL of EA were added. The organic layer was concentrated, crude product was purified by prep-HPLC to give 4 mg of the title compound.

후처리

  1. customconsumption of 2-bromo-5,6-dimethyl-8-propyl-3-thia-1,4,7,8a-tetraaza-as-indacene
  2. customAfter removal of the solvent under reduced pressure, 5 mL of water and 10 mL of EA
  3. additionwere added
  4. concentrationThe organic layer was concentrated
  5. customcrude product was purified by prep-HPLC

출처 및 근거

ORD 기록
ord-4f4d8dcc008a4fd79e479f0a0dab0242
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09388180B2

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