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Hydrochloric Acid → HCID 13671866、化合物

HRID 1655320
ノート
印刷プレビュー

反応式

HRID 1655320 の反応式
[NH2:1][CH:2]([CH2:11][CH2:12][CH:13]([CH3:15])[CH3:14])[CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4].[Cl:16][CH2:17][CH2:18][CH2:19][N:20]1[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1.[ClH:26]>C(O)C>[ClH:16].[ClH:26].[CH3:14][CH:13]([CH3:15])[CH2:12][CH2:11][CH:2]([NH:1][CH2:17][CH2:18][CH2:19][N:20]1[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1)[CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4]
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 3

HCID 313Hydrochloric AcidHCID 79625Piperidine, 1-(3-chloropropyl)-HCID 13671865HCID 13671865、化合物

生成物 1

HCID 13671866HCID 13671866、化合物収率 33%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of (1RS,2SR)-2-amino-5-methyl-1-phenylhexan-1-ol (415 mg, 2 mmol) and 1-(3-chloropropyl)piperidine (324 mg, 2 mmol) was melted at 70° C. in a nitrogen atmosphere. The mixture was heated at 110° to 120° C. for 3 hours. After being cooled, the reaction mixture was dissolved with heating in ethanol, followed by addition of concentrated hydrochloric acid (0.2 ml). After the mixture was cooled, precipitated crystals were collected by filtration and washed with ethanol. The crystals were recrystallized from ethanol to obtain 0.27 g of the title compound as white crystals (yield: 33%).

後処理

  1. temperatureThe mixture was heated at 110° to 120° C. for 3 hours
  2. temperatureAfter being cooled
  3. dissolutionthe reaction mixture was dissolved
  4. temperatureAfter the mixture was cooled
  5. customprecipitated crystals
  6. filtrationwere collected by filtration
  7. washwashed with ethanol
  8. customThe crystals were recrystallized from ethanol

出典と根拠

ORDレコード
ord-7618965cde3a48718346dd9085f10d57
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05250546

反応ノート

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