Ammonia → HCID 10243640、化合物

HRID 1885366ノート

反応式

HRID 1885366 の反応式
[NH3:1].[NH2:2][C:3]1[N:11]=[C:10]2[C:6]([N:7]=[CH:8][N:9]2[C@H:12]2[CH2:16][C@@H:15]([CH2:17][OH:18])[CH:14]=[CH:13]2)=[C:5](Cl)[N:4]=1>CO>[NH2:2][C:3]1[N:11]=[C:10]2[C:6]([N:7]=[CH:8][N:9]2[C@H:12]2[CH2:16][C@@H:15]([CH2:17][OH:18])[CH:14]=[CH:13]2)=[C:5]([NH2:1])[N:4]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 11777654(1R,4S)-4-(2-Amino-6-chloro-9H-purin-9-yl)-2-cyclopentene-1-methanol

生成物 1

HCID 10243640HCID 10243640、化合物収率 80%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
75 °C

実験手順

Liquid ammonia is passed into a solution of cis-(±)-2-amino-6-chloro-9-[4-(hydroxymethyl)-2-cyclopenten-1-yl]-9H-purine (0.265 g, 1 mmol) in methanol (10 mL) at -80° C. in a bomb. The bomb is sealed and heated at 75° C. for 48 hours. The bomb is cooled to room temperature and the ammonia and methanol are evaporated. The residue is purified by silica gel chromatography using 15:1 chloroform methanol as eluent to give cis-(±)-2,6-diamino-9-[4-(hydroxymethyl)-2-cyclo-penten-1-yl]-9H-purine (0.196 g, 80%). M.pt. 152°-155° C. MS (30 ev, 200° C.): m/e 246 (M+), 229 (M+-17), 216 (M+-30).

後処理

  1. customThe bomb is sealed
  2. temperatureThe bomb is cooled to room temperature
  3. customthe ammonia and methanol are evaporated
  4. customThe residue is purified by silica gel chromatography

出典と根拠

ORDレコード
ord-04bc2087409a45caa590302b58a00f49
出典データセット
uspto-grants-1992_09
特許番号
US05144034

反応ノート

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