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Sodium hydride → tert-butyl N-(4-[[6-(propan-2-yl)thieno[2,3-d]pyrimidin-4-yl]oxy]cyclohexyl)carbamate

HRID 525070
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HRID 525070 반응식
[OH:1][CH:2]1[CH2:7][CH2:6][CH:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:4][CH2:3]1.[H-].[Na+].Cl[C:19]1[C:20]2[CH:27]=[C:26]([CH:28]([CH3:30])[CH3:29])[S:25][C:21]=2[N:22]=[CH:23][N:24]=1>O1CCCC1>[CH3:30][CH:28]([C:26]1[S:25][C:21]2[N:22]=[CH:23][N:24]=[C:19]([O:1][CH:2]3[CH2:7][CH2:6][CH:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:12])([CH3:14])[CH3:13])[CH2:4][CH2:3]3)[C:20]=2[CH:27]=1)[CH3:29]
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참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 1514287cis-4-(tert-Butoxycarbonylamino)cyclohexanolHCID 27576274-Chloro-6-isopropylthieno(2,3-d)pyrimidine

생성물 1

HCID 68109905tert-butyl N-(4-[[6-(propan-2-yl)thieno[2,3-d]pyrimidin-4-yl]oxy]cyclohexyl)carbamate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a 100-mL 3-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen was placed a solution of tert-butyl N-(4-hydroxycyclohexyl)carbamate (3.3 g, 15.33 mmol, 1.10 equiv) in tetrahydrofuran (20 mL). This was followed by the addition of sodium hydride (800 mg, 33.33 mmol, 2.36 equiv) in portions at 0-5° C. The resulting solution was stirred for 2.5 h at room temperature. To this was added a solution of commercially available 4-chloro-6-(propan-2-yl)thieno[2,3-d]pyrimidine (3.0 g, 14.10 mmol, 1.00 equiv) in tetrahydrofuran (10 mL) at 5-10° C. The resulting solution was stirred overnight at room temperature. The reaction mixture was cooled to 5-10° C. with a water/ice bath. The reaction was then quenched by the addition of 100 mL of water. The resulting mixture was concentrated under vacuum. The solids were collected by filtration. This resulted in 4.8 g (87%) of tert-butyl N-(4-[[6-(propan-2-yl)thieno[2,3-d]pyrimidin-4-yl]oxy]cyclohexyl)carbamate as a yellow solid. MS: m/z 392 (M+H)+.

후처리

  1. customTo a 100-mL 3-necked round-bottom flask purged
  2. temperaturemaintained with an inert atmosphere of nitrogen
  3. stirringThe resulting solution was stirred overnight at room temperature
  4. temperatureThe reaction mixture was cooled to 5-10° C. with a water/ice bath
  5. customThe reaction was then quenched by the addition of 100 mL of water
  6. concentrationThe resulting mixture was concentrated under vacuum
  7. filtrationThe solids were collected by filtration
  8. customThis resulted in 4.8 g (87%) of tert-butyl N-(4-[[6-(propan-2-yl)thieno[2,3-d]pyrimidin-4-yl]oxy]cyclohexyl)carbamate as a yellow solid

출처 및 근거

ORD 기록
ord-6fc88b6284814b10aadcbd742fb5bdad
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09340554B2

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