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Water → 2-(4-Methoxy-benzyl)-6-((1S,3S)-3-amino-cyclopentyloxy)-2H-isoquinolin-1-one

HRID 402535
ノート
印刷プレビュー

反応式

HRID 402535 の反応式
[H-].[Na+].[NH2:3][C@H:4]1[CH2:8][CH2:7][C@H:6]([OH:9])[CH2:5]1.F[C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][CH:20]=1)[C:17](=[O:21])[N:16]([CH2:22][C:23]1[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][CH:24]=1)[CH:15]=[CH:14]2.O>CC(N(C)C)=O>[CH3:30][O:29][C:26]1[CH:25]=[CH:24][C:23]([CH2:22][N:16]2[CH:15]=[CH:14][C:13]3[C:18](=[CH:19][CH:20]=[C:11]([O:9][C@H:6]4[CH2:7][CH2:8][C@H:4]([NH2:3])[CH2:5]4)[CH:12]=3)[C:17]2=[O:21])=[CH:28][CH:27]=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

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 42614395(1S,3S)-3-Aminocyclopentan-1-olHCID 598182606-Fluoro-2-[(4-methoxyphenyl)methyl]isoquinolin-1-one

生成物 1

HCID 592248392-(4-Methoxy-benzyl)-6-((1S,3S)-3-amino-cyclopentyloxy)-2H-isoquinolin-1-one収率 49%

試薬・触媒・溶媒 1

HCID 31374
Dimethylacetamide
溶媒
3 回

反応条件

温度
80 °C

実験手順

106 mg (4.20 mmol) of sodium hydride (95%) were suspended in 3 mL of dimethyl acetamide and 193 mg (1.40 mmol) of (1S,3S)-3-amino-cyclopentanol (34), dissolved in 1 mL of dimethyl acetamide, were added dropwise. After 1 h, 402 mg (1.42 mmol) of 2-(4-methoxy-benzyl)-6-fluoro-2H-isoquinolin-1-one (9), dissolved in another 3 mL of dimethyl acetamide, were added. The reaction mixture was stirred at 80° C. until the reaction was complete. The mixture was poured into water, extracted three times with a mixture of dichloromethane and 2-propanol (3:1) and the combined organic layers were evaporated. Water was added and the crude product was subjected to lyophilization to remove remainders of dimethyl acetamide. The obtained crude product was purified by silica gel chromatography to yield 250 mg of the title compound (39). Rt=1.20 min (Method E). Detected mass: 365.2 (M+H+).

後処理

  1. additionwere added dropwise
  2. additionwere added
  3. extractionextracted three times
  4. additionwith a mixture of dichloromethane and 2-propanol (3:1)
  5. customthe combined organic layers were evaporated
  6. additionWater was added
  7. customto remove remainders of dimethyl acetamide
  8. customThe obtained crude product
  9. customwas purified by silica gel chromatography

出典と根拠

ORDレコード
ord-781560f9d9294b6b808b054dca68a86f
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08742116B2

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