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Hydrochloric Acid → Methyl {1-[(2R)-2-{[(4-fluorophenyl)sulfonyl](methyl)amino}-4-hydroxybutyl]-1H-pyrrolo[2,3-b]pyridin-3-yl}acetate

HRID 1036636
ノート
印刷プレビュー

反応式

HRID 1036636 の反応式
C[Si]([N-][Si](C)(C)C)(C)C.[Na+].[NH:11]1[C:15]2=[N:16][CH:17]=[CH:18][CH:19]=[C:14]2[C:13]([CH2:20][C:21]([O:23][CH3:24])=[O:22])=[CH:12]1.[Si]([O:32][CH2:33][CH2:34][C@@H:35]1[CH2:37][N:36]1[S:38]([C:41]1[CH:46]=[CH:45][C:44]([F:47])=[CH:43][CH:42]=1)(=[O:40])=[O:39])(C(C)(C)C)(C)C.I[CH3:49].Cl>CN(C=O)C>[F:47][C:44]1[CH:45]=[CH:46][C:41]([S:38]([N:36]([CH3:49])[C@H:35]([CH2:34][CH2:33][OH:32])[CH2:37][N:11]2[C:15]3=[N:16][CH:17]=[CH:18][CH:19]=[C:14]3[C:13]([CH2:20][C:21]([O:23][CH3:24])=[O:22])=[CH:12]2)(=[O:40])=[O:39])=[CH:42][CH:43]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 6328Methyl iodide2 回HCID 2724254Sodium bis(trimethylsilyl)amideHCID 25067325Methyl 2-(1H-pyrrolo[2,3-b]pyridin-3-yl)acetateHCID 58399169(2R)-2-(2-{[tert-butyl(dimethyl)silyl]oxy}ethyl)-1-[(4-fluoro-phenyl)sulfonyl]aziridine

生成物 1

HCID 86762092
Methyl {1-[(2R)-2-{[(4-fluorophenyl)sulfonyl](methyl)amino}-4-hydroxybutyl]-1H-pyrrolo[2,3-b]pyridin-3-yl}acetate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

実験手順

To a stirred solution of NaHMDS (177.22 g, 966 mmol) in DMF (600 ml) at −10° C. was added a solution of methyl 1H-pyrrolo[2,3-b]pyridin-3-ylacetate (197.98 g, 969 mmol) in DMF (1000 ml) over 15 min., and stirring continue at that temperature for 2 hours. To the anion was added a solution of (2R)-2-(2-{[tert-butyl(dimethyl)silyl]oxy}ethyl)-1-[(4-fluoro-phenyl)sulfonyl]aziridine (288 g, 801 mmol) in DMF (1000 ml) over 1 hour. The reaction mixture was stirred for 1 hour at −10° C. Iodomethane (125.0 ml, 1999 mmol) was added at −10° C. and the reaction was stirred for 1.5 hour. Another aliquot of iodomethane (20 mL) was then added and the reaction was stirred for 30 more minutes. 3N HCl (1800 ml, 5400 mmol) was added slowly at −10° C. and the reaction was stirred for an additional hour. The reaction was quenched by pouring into saturated sodium bicarbonate solution (4 L) and ethyl acetate (4 L). The pH was still acidic so additional solid sodium bicarbonate was added. The layers were separated and the organic layer washed with ½ brine (1×4 L) and (1×2 L).

後処理

  1. stirringThe reaction mixture was stirred for 1 hour at −10° C
  2. stirringthe reaction was stirred for 1.5 hour
  3. stirringthe reaction was stirred for 30 more minutes
  4. stirringthe reaction was stirred for an additional hour
  5. customThe reaction was quenched
  6. additionby pouring into saturated sodium bicarbonate solution (4 L) and ethyl acetate (4 L)
  7. additionwas added
  8. customThe layers were separated
  9. washthe organic layer washed with ½ brine (1×4 L) and (1×2 L)

出典と根拠

ORDレコード
ord-c1e53db69bce4ff386db4631a4d34f4f
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546422B2

反応ノート

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