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Methanol → Ly-2940094

HRID 1517605
ノート
印刷プレビュー

反応式

HRID 1517605 の反応式
[Cl:1][C:2]1[S:6][C:5]2[C:7]3([O:28][CH2:29][C:30]([F:32])([F:31])[C:4]=2[CH:3]=1)[CH2:12][CH2:11][N:10]([CH2:13][C:14]1[C:15]([CH3:27])=[N:16][N:17]([C:19]2[C:24]([CH:25]=[O:26])=[CH:23][CH:22]=[CH:21][N:20]=2)[CH:18]=1)[CH2:9][CH2:8]3.[BH4-].[Na+].CO>ClCCl>[Cl:1][C:2]1[S:6][C:5]2[C:7]3([O:28][CH2:29][C:30]([F:32])([F:31])[C:4]=2[CH:3]=1)[CH2:12][CH2:11][N:10]([CH2:13][C:14]1[C:15]([CH3:27])=[N:16][N:17]([C:19]2[C:24]([CH2:25][OH:26])=[CH:23][CH:22]=[CH:21][N:20]=2)[CH:18]=1)[CH2:9][CH2:8]3
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 4311764Sodium borohydrideHCID 582685962-[4-[(2-Chloro-4,4-difluoro-spiro[5H-thieno[2,3-c]pyran-7,4'-piperidine]-1'-yl)methyl]-3-methyl-pyrazol-1-yl]pyridine-3-carbaldehyde

生成物 1

HCID 52914971Ly-2940094収率 95.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2-[4-[(2-chloro-4,4-difluoro-spiro[5H-thieno[2,3-c]pyran-7,4′-piperidine]-1′-yl)methyl]-3-methyl-pyrazol-1-yl]pyridine-3-carbaldehyde (12.50 g, 26.10 mmol) in dichloromethane (125 mL) at 0° C. is added sodium borohydride (0.395 g, 10.44 mmol) and methanol (37.50 mL). The ice bath is removed and the reaction is stirred at room temperature for 30 min. Water (50 mL) is added and the mixture is concentrated to half volume resulting in a white sticky solid precipitate. Dichloromethane (100 mL) is added and the biphasic mixture is separated. The organic layer is washed with water (50 mL), dried over sodium sulfate and concentrated to half volume (around 100 mL). Methyl tert-butyl ether (100 mL) is added and the solution is concentrated to provide a precipitate. The solid is filtered and dried under vacuum to give 12 g of [2-[4-[(2-chloro-4,4-difluoro-spiro[5H-thieno[2,3-c]pyran-7,4′-piperidine]-1′-yl)methyl]-3-methyl-pyrazol-1-yl]-3-pyridyl]methanol. MS (m/z): 481 (M+1).

後処理

  1. customThe ice bath is removed
  2. additionWater (50 mL) is added
  3. concentrationthe mixture is concentrated to half volume
  4. customresulting in a white sticky solid precipitate
  5. customthe biphasic mixture is separated
  6. washThe organic layer is washed with water (50 mL)
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated to half volume (around 100 mL)
  9. additionMethyl tert-butyl ether (100 mL) is added
  10. concentrationthe solution is concentrated
  11. customto provide a precipitate
  12. filtrationThe solid is filtered
  13. customdried under vacuum

出典と根拠

ORDレコード
ord-89d1e9fc972842fc878c8e3188405b7c
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08232289B2

反応ノート

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