Hydrochloric Acid → HCID 13671877、化合物

HRID 1655322ノート

反応式

HRID 1655322 の反応式
[NH2:1][CH:2]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4].[Cl:17][CH2:18][CH2:19][CH2:20][N:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1.[ClH:27].C(OCC)(=O)C>C(O)C.CCCCCC>[ClH:17].[ClH:27].[C:5]1([CH:3]([OH:4])[CH:2]([NH:1][CH2:18][CH2:19][CH2:20][N:21]2[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]2)[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 462682-Amino-1-phenyloctan-1-olHCID 79625Piperidine, 1-(3-chloropropyl)-

生成物 1

HCID 13671877HCID 13671877、化合物収率 59%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8058Hexane溶媒

実験手順

A mixture of (1RS,2RS)-2-amino-1-phenyloctan-1-ol (1.77 g, 8 mmol) and 1-(3-chloropropyl)piperidine (1.29 g, 8 mmol) was melted at 70° C. in a nitrogen atmosphere. The mixture was then heated at 110° to 120° C. for 3 hours. The reaction mixture was dissolved with heating in ethanol, followed by addition of concentrated hydrochloric acid (0.67 ml). Ethyl acetate was added and the resulting mixture was allowed to stand. Precipitated crystals were collected by filtration and washed with ethyl acetate and then with hexane to obtain 1.96 g of the title compound as white crystals (yield: 59%).

後処理

  1. temperatureThe mixture was then heated at 110° to 120° C. for 3 hours
  2. dissolutionThe reaction mixture was dissolved
  3. customPrecipitated crystals
  4. filtrationwere collected by filtration
  5. washwashed with ethyl acetate

出典と根拠

ORDレコード
ord-33defaaa5d474bbdae105d28b5990846
出典データセット
uspto-grants-1993_10
特許番号
US05250546

反応ノート

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