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Sodium borohydride → HCID 12508669、化合物

HRID 1633330
ノート
印刷プレビュー

反応式

HRID 1633330 の反応式
[CH3:1][C:2]12[CH:14]([CH2:15][CH3:16])[N:6]([CH:7]([CH2:12][CH3:13])[NH:8][CH:9]1[CH2:10][CH3:11])[CH:5]([CH2:17][CH3:18])[N:4]=[CH:3]2.[BH4-].[Na+]>[OH-].[Na+].C(O)C>[CH2:3]([C:2]1([CH3:1])[CH:9]([CH2:10][CH3:11])[NH:8][CH:7]([CH2:12][CH3:13])[NH:6][CH:14]1[CH2:15][CH3:16])[NH:4][CH2:5][CH2:17][CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 4311764Sodium borohydrideHCID 12508656HCID 12508656、化合物

生成物 1

HCID 12508669HCID 12508669、化合物収率 90.3%

試薬・触媒・溶媒 2

HCID 14798Sodium Hydroxide触媒HCID 702Ethanol溶媒

実験手順

To a mixture of 70 grams of 5-methyl-2,6,8,9-tetraethyl-1,3,7-triazabicyclo (3,3,1) non-3-ene, 0.5 grams of sodium hydroxide, and 190 grams of ethanol was added, with stirring, over a 1/2 hour period 9 grams of sodium borohydride. The mixture was stirred for 20 hours at ambient temperature. The ethanol was removed under diminished pressure and the resulting product was added to water and extracted with ether. The ethereal solution, after drying over anh. MgSO4, was evaporated under diminished pressure to yield 64.2 grams of 5-(2-azapentyl)-5-methyl-2,4,6-triethylhexahydropyrimidine, b.p. 138°-150° C./20 torr.

後処理

  1. additionwas added
  2. customThe ethanol was removed under diminished pressure
  3. additionthe resulting product was added to water
  4. extractionextracted with ether
  5. dry with materialThe ethereal solution, after drying over anh. MgSO4
  6. customwas evaporated under diminished pressure

出典と根拠

ORDレコード
ord-5641177489ca4d79bf9681b34f631b0a
出典データセット
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04480095

反応ノート

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