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HCID 70466244、化合物 → 1-(6-amino-9H-purin-9-yl)-1,3-dideoxy-3-amino-beta-D-ribofuranuronic acid monohydrate

HRID 1633320
ノート
印刷プレビュー

反応式

HRID 1633320 の反応式
O.Cl.Cl.[NH2:4][C:5]1[N:13]=[CH:12][N:11]=[C:10]2[C:6]=1[N:7]=[CH:8][N:9]2[C@@H:14]1[O:19][C@H:18]([C:20]([OH:22])=[O:21])[C@@H:17]([NH:23]C(=O)[C@H](CC2C=CC(OC)=CC=2)N)[C@H:15]1[OH:16]>[OH-].[Na+]>[OH2:16].[NH2:4][C:5]1[N:13]=[CH:12][N:11]=[C:10]2[C:6]=1[N:7]=[CH:8][N:9]2[C@@H:14]1[O:19][C@H:18]([C:20]([OH:22])=[O:21])[C@@H:17]([NH2:23])[C@H:15]1[OH:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 70466244HCID 70466244、化合物

生成物 1

HCID 704655221-(6-amino-9H-purin-9-yl)-1,3-dideoxy-3-amino-beta-D-ribofuranuronic acid monohydrate収率 165.7%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A mixture of 1-(6-amino-9H-purin-9-yl)-1,3-dideoxy-3-(O-methyl-L-tyrosylamino)-β-D-ribofuranuronic acid dihydrochloride monohydrate (5.48 g) prepared in Example 98 in 1N methanolic sodium hydroxide solution (1000 ml) was heated under reflux for 20 hours. The reaction mixture was evaporated and the residue was neutralized with concentrated hydrochloric acid. The aqueous solution was subjected to column chromatography on a non-ionic adsorption resin "HP-20" (trade mark, Mitsubishi Chemical Industries Ltd.) (500 ml). The elution was carried out with water, and the eluate was concentrated, stood overnight. The resulting precipitates were collected, washed with water, and dried to give 1-(6-amino-9H-purin-9-yl)-1,3-dideoxy-3-amino-β-D-ribofuranuronic acid monohydrate (2.47 g).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 20 hours
  3. customThe reaction mixture was evaporated
  4. washThe elution
  5. concentrationthe eluate was concentrated
  6. customThe resulting precipitates
  7. customwere collected
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-64d413c61d0145bd8e58f9b00d9a451f
出典データセット
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04479942

反応ノート

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