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Dimethyl Sulfoxide → 2-{4-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]cyclohexyl}acetaldehyde

HRID 51598
ノート
印刷プレビュー

反応式

HRID 51598 の反応式
CS(C)=O.C(Cl)(=O)C(Cl)=O.[NH2:11][C:12]1[C:13]2[C:20]([C:21]3[CH:26]=[CH:25][C:24]([O:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)=[CH:23][CH:22]=3)=[CH:19][N:18]([CH:34]3[CH2:39][CH2:38][CH:37]([CH2:40][CH2:41][OH:42])[CH2:36][CH2:35]3)[C:14]=2[N:15]=[CH:16][N:17]=1.C(N(CC)CC)C.C(=O)(O)[O-].[Na+]>ClCCl>[NH2:11][C:12]1[C:13]2[C:20]([C:21]3[CH:22]=[CH:23][C:24]([O:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)=[CH:25][CH:26]=3)=[CH:19][N:18]([CH:34]3[CH2:35][CH2:36][CH:37]([CH2:40][CH:41]=[O:42])[CH2:38][CH2:39]3)[C:14]=2[N:15]=[CH:16][N:17]=1
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

7

反応物 5

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 516892Sodium BicarbonateHCID 227362622-{4-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]cyclohexyl}-1-ethanol

生成物 1

HCID 227361722-{4-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]cyclohexyl}acetaldehyde
収率 52.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-40 °C

実験手順

Dimethylsulfoxide (0.040 g, 0.51 mmol) was added into a solution of oxalyl chloride (0.033 g, 0.26 mmol) in dichloromethane (3 mL) at −78° C. The mixture was allowed to warm up to −40° C. and stirred for 15 minutes followed by cooling down to −78° C. again. 2-{4-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]cyclohexyl}-1-ethanol (0.10 g, 0.23 mmol) was added followed by triethylamine (0.12 mg, 1.165 mmol). The mixture was allowed to warm up to 0° C. and saturated aqueous sodium bicarbonate solution (10 mL) was added to quench the reaction. The organic layer was separated from the aqueous layer and washed with 10% aqueous sodium hydorgensulfate solution (4 mL), saturated aqueous sodium bicarbonate solution (4 mL) and saturated aqueous sodium chloride (4 mL). The organic layer was dried over magnesium sulfate and the solvent was removed under reduced pressure. The residue was purified by flash chromatography on silica gel using methanol/dichloromethane(5:95) as a mobile phase to yield 2-{4-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]cyclohexyl}acetaldehyde (0.053 g, 0.12 mmol) as a white solid: 1H NMR (CDCl3, 400 MHz) δ 9.81(s, 1H), 8.33(s, 1H), 7.68(m, 1H), 7.43(d, 2H), 7.38(t, 2H), 7.15(t, 1H), 7.07(m, 4H), 5.14 (br, 2H), 4.72(m, 1H), 2.63-1.72(m, 11H); TLC (methanol/dichloromethane=5:95) Rf 0.41. MS: MH+ 427.

後処理

  1. temperatureby cooling down to −78° C. again
  2. temperatureto warm up to 0° C.
  3. customto quench
  4. customthe reaction
  5. customThe organic layer was separated from the aqueous layer
  6. washwashed with 10% aqueous sodium hydorgensulfate solution (4 mL), saturated aqueous sodium bicarbonate solution (4 mL) and saturated aqueous sodium chloride (4 mL)
  7. dry with materialThe organic layer was dried over magnesium sulfate
  8. customthe solvent was removed under reduced pressure
  9. customThe residue was purified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-5f31a854d16f4008a75eab26fa7c0033
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06713474B2

反応ノート

読み込み中…

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