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Sodium Carbonate → 6-((7S)-hydroxy-6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-7-yl)-N-methyl-2-naphthamide

HRID 922722
ノート
印刷プレビュー

反応式

HRID 922722 の反応式
O[C@@:2]([C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][CH:20]=1)[CH:17]=[C:16]([C:21]([NH:23][CH3:24])=[O:22])[CH:15]=[CH:14]2)([C:6]1[N:7]=[CH:8][NH:9][CH:10]=1)[CH2:3][CH2:4]O.C(N(C(C)C)C(C)C)C.CS(Cl)(=O)=[O:36].C(=O)([O-])[O-].[Na+].[Na+]>O1CCCC1.O.C(OCC)(=O)C>[OH:36][C:10]1[N:9]=[CH:8][N:7]2[CH2:4][CH2:3][C@@H:2]([C:11]3[CH:12]=[C:13]4[C:18](=[CH:19][CH:20]=3)[CH:17]=[C:16]([C:21]([NH:23][CH3:24])=[O:22])[CH:15]=[CH:14]4)[C:6]=12
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

8

反応物 4

HCID 10340Sodium CarbonateHCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 178485275HCID 178485275、化合物

生成物 1

HCID 666510376-((7S)-hydroxy-6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-7-yl)-N-methyl-2-naphthamide収率 58.1%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

To a solution of 6-[(1S)-1,3-dihydroxy-1-(1H-imidazol-4-yl)propyl]-N-methyl-2-naphthamide (1.0 g, 3.1 mmol) in tetrahydrofuran (100 mL) were added N-ethyldiisopropylamine (2.39 g, 18.4 mmol) and methanesulfonyl chloride (2.11 g, 18.4 mmol) at room temperature. The mixture was stirred at the same temperature for 3 hr. To the reaction mixture was added a solution of sodium carbonate (1.31 g, 12.3 mmol) in water (3 mL). The mixture was heated to 60° C. and stirred for 5 hr. After the reaction mixture was allowed to cool to room temperature, ethyl acetate (25 mL) was added thereto. The organic layer was separated and concentrated under reduced pressure. Methanol (16.7 mL) and water (6.4 mL) were added to the residue. The mixture was heated to 65° C., and activated carbon (45 mg) was added thereto. After stirring at the same temperature for 30 min, the activated carbon was filtered off and washed with methanol (1.1 mL). Water (6.4 mL) was added to the filtrate at 55° C. The resulting mixture was allowed to cool to room temperature and stirred for 30 min. To the mixture was added water (6.4 mL) at the same temperature, and the mixture was stirred for 2 hr. The mixture was cooled to 0° C. and stirred for 2 hr. The obtained precipitated crystals were collected by filtration, washed with 45% aqueous methanol (3 mL), and dried under reduced pressure to give 6-((7S)-hydroxy-6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-7-yl)-N-methyl-2-naphthamide (540 mg, 1.8 mmol). yield 57%.

後処理

  1. stirringstirred for 5 hr
  2. temperatureto cool to room temperature
  3. customThe organic layer was separated
  4. concentrationconcentrated under reduced pressure
  5. additionMethanol (16.7 mL) and water (6.4 mL) were added to the residue
  6. temperatureThe mixture was heated to 65° C.
  7. additionactivated carbon (45 mg) was added
  8. stirringAfter stirring at the same temperature for 30 min
  9. filtrationthe activated carbon was filtered off
  10. washwashed with methanol (1.1 mL)
  11. additionWater (6.4 mL) was added to the filtrate at 55° C
  12. temperatureto cool to room temperature
  13. stirringstirred for 30 min
  14. additionTo the mixture was added water (6.4 mL) at the same temperature
  15. stirringthe mixture was stirred for 2 hr
  16. temperatureThe mixture was cooled to 0° C.
  17. stirringstirred for 2 hr
  18. customThe obtained precipitated crystals
  19. filtrationwere collected by filtration
  20. washwashed with 45% aqueous methanol (3 mL)
  21. customdried under reduced pressure

出典と根拠

ORDレコード
ord-788ea0540b284ec39b05d755f95197ba
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278938B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート