3-Hydroxypiperidine → HCID 178511975、化合物

HRID 1464112ノート

反応式

HRID 1464112 の反応式
[C:1]1([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8]#[N:9].[OH:16][CH:17]1[CH2:22][CH2:21][CH2:20][NH:19][CH2:18]1>C(O)C>[C:1]1([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8]([N:19]1[CH2:20][CH2:21][CH2:22][CH:17]([OH:16])[CH2:18]1)=[NH:9]

参加物

4

反応物 2

HCID 232933-HydroxypiperidineHCID 190892212-Biphenylylcyanamide

生成物 1

HCID 178511975HCID 178511975、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-biphenylylcyanamide (4 g), 3-hydroxypiperidine (2.5 g) and ethanol (30 ml) was heated at 90°-95° C. for 8 hours to give a brown solid which was purified by chromatography on an aluminia column eluted successively with hexane, 1:4, 2:3, 3:2 and 4:1 mixtures of dichloromethane and hexane and then a 99:1 mixture of dichloromethane and methanol to yield a solid which was recrystallised from ethyl acetate to give N-(2-biphenylyl)-3-hydroxypiperidine-1-carboxamidine (m.p. 144°-145° C.).

後処理

  1. temperaturewas heated at 90°-95° C. for 8 hours
  2. customto give a brown solid which
  3. customwas purified by chromatography on an aluminia column
  4. washeluted successively with hexane, 1:4, 2:3, 3:2 and 4:1 mixtures of dichloromethane and hexane
  5. additiona 99:1 mixture of dichloromethane and methanol
  6. customto yield a solid which
  7. customwas recrystallised from ethyl acetate

出典と根拠

ORDレコード
ord-db3a398202d94ce8bee3de34aab6cc89
出典データセット
uspto-grants-1994_04
特許番号
US05302720

反応ノート

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