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Sulfamide → HCID 46852046, 화합물

HRID 241653
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HRID 241653 반응식
[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([CH2:17][CH:18]4[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]4)(=[O:16])=[O:15])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:24][C:25]([CH3:28])([CH3:27])[CH3:26])[CH2:3][CH2:2]1.[S:29](N)([NH2:32])(=[O:31])=[O:30]>O1CCOCC1>[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([CH2:17][CH:18]4[CH2:19][CH2:20][N:21]([S:29]([NH2:32])(=[O:31])=[O:30])[CH2:22][CH2:23]4)(=[O:15])=[O:16])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:24][C:25]([CH3:28])([CH3:27])[CH3:26])[CH2:2][CH2:3]1
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참가 물질

4

반응물 2

HCID 82267SulfamideHCID 58513582HCID 58513582, 화합물

생성물 1

HCID 46852046HCID 46852046, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

The mixture of 1-(cyclopropylmethyl)-2-(2,2-dimethylpropyl)-5-[(piperidin-4-ylmethane)sulfonyl]-1,3-benzodiazole (STEP D of Example 5, 25 mg, 0.062 mmol), sulfamide (15 mg, 0.16 mmol)and 1,4-dioxane was refluxed for 6 h. The reaction mixture was concentrated in vacuo and extracted with ethyl acetate (20 mL) and water (30 mL). The organic layer was washed with water (20 mL) and brine (15 mL), dried over magnesium sulfate. The crude product (27 mg) was purified by prep LC-MS(“process A”).

후처리

  1. temperaturewas refluxed for 6 h
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. extractionextracted with ethyl acetate (20 mL) and water (30 mL)
  4. washThe organic layer was washed with water (20 mL) and brine (15 mL)
  5. dry with materialdried over magnesium sulfate
  6. customThe crude product (27 mg) was purified by prep LC-MS(“process A”)

출처 및 근거

ORD 기록
ord-e40437972a6a4f05b9909595a40c0178
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08653063B2

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