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Sodium Azide → Ethyl (1-benzyl-2-methyl-1H-pyrrolo[2,3-b]pyridin-4-yloxy)acetate

HRID 1445928
ノート
印刷プレビュー

反応式

HRID 1445928 の反応式
C(N1C2C=CN[C:12](=[O:17])[C:11]=2C=C1C)C1C=CC=CC=1.C(N1C(C)=CC=C1C=C[C:34](O)=[O:35])C1C=CC=CC=1.[CH2:37]([N:44]1[C:48]2=[N:49][CH:50]=[CH:51][C:52]([O:53][CH3:54])=[C:47]2[CH:46]=[C:45]1[CH3:55])[C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1.[N-]=[N+]=[N-].[Na+]>CC(C)=O.O.C(N(CC)CC)C>[CH2:37]([N:44]1[C:48]2=[N:49][CH:50]=[CH:51][C:52]([O:53][CH2:54][C:34]([O:17][CH2:12][CH3:11])=[O:35])=[C:47]2[CH:46]=[C:45]1[CH3:55])[C:38]1[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=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

8

反応物 4

HCID 33557Sodium AzideHCID 588959911-Benzyl-4-methoxy-2-methyl-1H-pyrrolo[2,3-b]pyridineHCID 591703201-Benzyl-2-methyl-1,5-dihydro-pyrrolo[3,2-c]pyridin-4-oneHCID 685492913-(1-Benzyl-5-methyl-1H-pyrrol-2-yl)-acrylic acid

生成物 1

HCID 58895970Ethyl (1-benzyl-2-methyl-1H-pyrrolo[2,3-b]pyridin-4-yloxy)acetate

試薬・触媒・溶媒 3

HCID 180
Acetone
溶媒
2 回
HCID 962Water溶媒
HCID 8471Triethylamine溶媒

反応条件

温度
0 °C

実験手順

1-Benzyl-2-methyl-1,5-dihydro-pyrrolo[3,2-c]pyridin-4-one, 9: 3-(1-Benzyl-5-methyl-1H-pyrrol-2-yl)-acrylic acid, 6 (26.72 g, 110.9 mmol) was dissolved in a dry acetone (1050 mL). To the suspension mixture triethylamine (35 mL) was added to form a clear solution. The reaction mixture was cooled to 0° C. and then to the cooled reaction mixture a solution of ethyl chlorofomate (30 mL, 304 mmol) in dry acetone (650 mL) was added dropwise over 1 hour. After addition the reaction mixture was stirred for 4 h at 0° C. Then to the reaction mixture was added dropwise the solution of sodium azide (14.52 g, 223 mmol) in H2O (175 mL) over 30 minutes. The reaction mixture was stirred at 0° C. for 2 h. The reaction mixture was poured into ice-water (1 L). Then the mixture was extracted with dichloromethane (3×1 L). The organic layers were combined and dried over MgSO4. The mixture was filtered and concentrated to afford a crude 8 as a yellow solid (32 g). To the mixture of diphenyl ether (175 mL) and tributylamine (31 mL) which was preheated to 205° C. was added dropwise the solution of crude 8 in diphenyl ether (250 mL) at 205° C. for 1 hour. After addition the mixture was stirred for another hour at 205° C. The mixture was cooled to room temperature and solid was formed. Diethyl ether (500 mL) was added into the reaction mixture to form more solid. The mixture was filtered and the solid was washed with diethyl ether to afford the product (8.81 g). The filtrate was concentrated and the residue was purified by silica gel chromatography (hexane to hexane:ethyl acetate, gradient 1:1 to 1:3; then methanol in dichloromethane, 1% to 5%) to afford 1-benzyl-2-methyl-1,5-dihydro-pyrrolo[3,2-c]pyridin-4-one, 9 as a yellow solid (4.7 g). Yield: 13.51 g, (51%)

後処理

  1. customto form a clear solution
  2. additionwas added dropwise over 1 hour
  3. additionAfter addition the reaction mixture
  4. stirringThe reaction mixture was stirred at 0° C. for 2 h
  5. extractionThen the mixture was extracted with dichloromethane (3×1 L)
  6. dry with materialdried over MgSO4
  7. filtrationThe mixture was filtered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-8d893ed141934537bba3bee0c48f7e1b
出典データセット
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07666898B2

反応ノート

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