Sodium Methoxide → 6-Acetyl-2-butyl-5,6,7,8-tetrahydro-pyrido-[4,3-d]pyrimidin-4(3H)-one

HRID 1198463

反応式

HRID 1198463 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][C:7](=O)[CH:6]([C:11]([O:13]CC)=O)[CH2:5]1)(=[O:3])[CH3:2].Cl.[C:17]([NH2:23])(=[NH:22])[CH2:18][CH2:19][CH2:20][CH3:21].C[O-].[Na+]>C(O)C.CO>[C:1]([N:4]1[CH2:9][CH2:8][C:7]2[N:22]=[C:17]([CH2:18][CH2:19][CH2:20][CH3:21])[NH:23][C:11](=[O:13])[C:6]=2[CH2:5]1)(=[O:3])[CH3:2]

参加物

6

反応物 3

HCID 10942334Sodium MethoxideHCID 11615174Pentanimidamide HydrochlorideHCID 12445847Ethyl 1-acetyl-4-oxo-3-piperidinecarboxylate

生成物 1

HCID 1360140346-Acetyl-2-butyl-5,6,7,8-tetrahydro-pyrido-[4,3-d]pyrimidin-4(3H)-one収率 96.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

A mixture of 1.5 g of ethyl 1-acetyl-4-oxo-3-piperidinecarboxylate and 1.0 g of valeramidine hydrochloride in 15 ml of anhydrous ethyl alcohol is treated with 7.5 ml of a 1M solution of sodium methoxide in methanol. The resulting mixture is stirred and heated at reflux for one hour. The reaction mixture is allowed to cool over 30 minutes then filtered. The filtrate is evaporated to a colorless syrup which is stirred with 50 ml of ether for 2 hours then filtered. The tacky cake is dried under high vacuum at 56° C. to afford 1.7 g of the desired product, m.p. 106°-113° C.

後処理

  1. temperatureheated
  2. temperatureat reflux for one hour
  3. temperatureto cool over 30 minutes
  4. filtrationthen filtered
  5. customThe filtrate is evaporated to a colorless syrup which
  6. stirringis stirred with 50 ml of ether for 2 hours
  7. filtrationthen filtered
  8. customThe tacky cake is dried under high vacuum at 56° C.

出典と根拠

ORDレコード
ord-2c365a98f2c74fdbbaf1488ebff5bce4
出典データセット
uspto-grants-1994_01
特許番号
US05281602

関連ノート

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