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Hydrazine hydrate (1:1) → 9-(3-Aminopropyl)-2-butoxy-8-methoxy-9H-purin-6-amine

HRID 2036348
ノート
印刷プレビュー

反応式

HRID 2036348 の反応式
[NH2:1][C:2]1[N:10]=[C:9]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([O:30][CH3:31])[N:6]2[CH2:16][CH2:17][CH2:18][N:19]1C(=O)C2C(=CC=CC=2)C1=O.O.NN>C(O)C>[NH2:19][CH2:18][CH2:17][CH2:16][N:6]1[C:5]([O:30][CH3:31])=[N:4][C:3]2[C:7]1=[N:8][C:9]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])=[N:10][C:2]=2[NH2:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 582909572-[3-(6-Amino-2-butoxy-8-methoxy-9H-purin-9-yl)propyl]-1H-isoindole-1,3(2H)-dione

生成物 1

HCID 231585469-(3-Aminopropyl)-2-butoxy-8-methoxy-9H-purin-6-amine収率 65.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-{3-[6-Amino-2-(butyloxy)-8-(methyloxy)-9H-purin-9-yl]propyl}-1H-isoindole-1,3(2H)-dione (6.06 g, 14.28 mmol) was dissolved in ethanol (60 ml) and hydrazine monohydrate (6.00 ml) was added and stirred at ambient temperature for 10 hours. The resultant mixture was concentrated under reduced pressure and the residue suspended in DCM (100 ml) and stirred for 1 hour. The suspension was filtered, and the filtered solid washed with DCM (10 ml). The filtrate and washings were washed with water (50 ml) and dried. The organic solution was concentrated under reduced pressure to give the title compound as an off-white solid (2.74 g).

後処理

  1. concentrationThe resultant mixture was concentrated under reduced pressure
  2. stirringstirred for 1 hour
  3. filtrationThe suspension was filtered
  4. washthe filtered solid washed with DCM (10 ml)
  5. washThe filtrate and washings were washed with water (50 ml)
  6. customdried
  7. concentrationThe organic solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-360a6d5f1aa141c2a2bf7d07b331b520
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08575181B2

反応ノート

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