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

HRID 1051430
ノート
印刷プレビュー

反応式

HRID 1051430 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4f4d8dcc008a4fd79e479f0a0dab0242
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09388180B2

反応ノート

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