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Sodium borohydride → HCID 90931501、化合物

HRID 1093230
ノート
印刷プレビュー

反応式

HRID 1093230 の反応式
[CH3:1][O:2][C:3](=[O:35])[NH:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[N:16]=[C:15]3[N:17]([CH:20]4[CH2:25][CH2:24][C:23](=[O:26])[CH2:22][CH2:21]4)[N:18]=[CH:19][C:14]3=[C:13]([N:27]3[CH2:33][CH:32]4[O:34][CH:29]([CH2:30][CH2:31]4)[CH2:28]3)[N:12]=2)=[CH:7][CH:6]=1.[BH4-].[Na+]>C1COCC1>[CH3:1][O:2][C:3](=[O:35])[NH:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[N:16]=[C:15]3[N:17]([CH:20]4[CH2:25][CH2:24][CH:23]([OH:26])[CH2:22][CH2:21]4)[N:18]=[CH:19][C:14]3=[C:13]([N:27]3[CH2:33][CH:32]4[O:34][CH:29]([CH2:30][CH2:31]4)[CH2:28]3)[N:12]=2)=[CH:9][CH:10]=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 4311764Sodium borohydrideHCID 91022940HCID 91022940、化合物

生成物 1

HCID 90931501HCID 90931501、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of methyl{4-[4-(8-oxa-3-azabicyclo[3.2.1]oct-3-yl)-1-(4-oxocyclohexyl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]phenyl}carbamate (63 mg) (0.13 mmol) in THF (2.0 mL) was added an excess of sodium borohydride. The mixture was stirred for 1 hr. at 50 C. The reaction was then cooled and quenched with water and extracted three times with EtOAc. Organics were dried (MgSO4) and concentrated in vacuo. The resulting oil was triturated with diethyl ether to give a white solid. The solid was filtered and washed the diethyl ether to give (44 mg) MS m/z=479.2 (M+H).

後処理

  1. temperatureThe reaction was then cooled
  2. customquenched with water
  3. extractionextracted three times with EtOAc
  4. dry with materialOrganics were dried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe resulting oil was triturated with diethyl ether
  7. customto give a white solid
  8. filtrationThe solid was filtered
  9. washwashed the diethyl ether
  10. customto give (44 mg)

出典と根拠

ORDレコード
ord-32a7d144ef7e4a5481da6539cd023bbd
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08129371B2

反応ノート

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