HCID 385229、化合物 → HCID 385226、化合物

HRID 1421879ノート

反応式

HRID 1421879 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:15][OH:16])[CH2:13][C:12](=[O:14])[CH2:11]2)[CH:5]=[C:4]([Cl:17])[N:3]=1.[BH4-].[Na+].Cl.C(O)C>C(O)C>[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:15][OH:16])[CH2:11][CH:12]([OH:14])[CH2:13]2)[CH:5]=[C:4]([Cl:17])[N:3]=1

参加物

5

反応物 3

HCID 385229HCID 385229、化合物HCID 4311764Sodium borohydrideHCID 21887872Ethanol hydrochloride

生成物 1

HCID 385226HCID 385226、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Amino-6-chloro-4-[[(1-hydroxymethyl-3-oxo-1-cyclobutyl)methyl]-amino]pyrimidine (2.21 g, 8.26 mmol) was dissolved in ethanol (80 ml) and sodium borohydride (0.31 g, 8.26 mmol) was added portionwise under ice-cooling. The mixture was stirred at room temperature for 30 minutes. The mixture was neutralized with hydrochloric acid-ethanol. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=100:7) to give white crystals (2.14 g, quantitative), m.p. 136-139° C. (ethyl acetate).

後処理

  1. temperaturecooling
  2. distillationThe solvent was distilled away under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (chloroform:methanol=100:7)
  4. customto give white crystals (2.14 g, quantitative), m.p. 136-139° C. (ethyl acetate)

出典と根拠

ORDレコード
ord-9368c8825f2046279f7fbb546fde140b
出典データセット
uspto-grants-2000_06
特許番号
US06080750

反応ノート

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