Hydrochloric Acid → HCID 22712048、化合物

HRID 352434

反応式

HRID 352434 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][CH3:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:16]1([CH:19]=O)[CH2:18][CH2:17]1.C([BH3-])#N.[Na+].Cl>CO>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH2:19][CH:16]2[CH2:18][CH2:17]2)[CH3:15])[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 123114CyclopropanecarboxaldehydeHCID 41361281-benzyl-N-methylpiperidin-4-amineHCID 5003444Sodium cyanoborohydride

生成物 1

HCID 22712048HCID 22712048、化合物収率 95%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
45 °C

実験手順

18.9 g of 1-benzyl-4-methylaminopiperidine in the form of the oil prepared in a) are taken up in 250 ml of methanol, combined with 8.3 g of cyclopropane carboxaldehyde and 11.3 g of sodium cyanoborohydride. The mixture is stirred for 5 hours at 40-50° C., then for about 16 hours at ambient temperature. It is then acidified with 2 N hydrochloric acid, evaporated to dryness in vacuo and the residue is taken up in water. It is washed with ether, made alkaline with concentrated sodium hydroxide solution and extracted with ether/ethyl acetate. The organic extract is dried over sodium sulphate and freed from solvents in vacuo. 22.7 g of 1-benzyl-4-(cyclopropylmethyl-methyl-amino)-piperidine are obtained as a yellowish oil.

後処理

  1. waitfor about 16 hours at ambient temperature
  2. customevaporated to dryness in vacuo
  3. washIt is washed with ether
  4. extractionextracted with ether/ethyl acetate
  5. extractionThe organic extract
  6. dry with materialis dried over sodium sulphate

出典と根拠

ORDレコード
ord-f8daccd7025a4cf39fdc5c8693be6b22
出典データセット
uspto-grants-2004_06
特許番号
US06747044B2

関連ノート

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