Diisopropylamine → HCID 68899458、化合物

HRID 523587ノート

反応式

HRID 523587 の反応式
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.[C:8]1(=[O:12])[CH2:11][CH2:10][CH2:9]1.C([Li])CCC.C(NC(C)C)(C)C>C1COCC1>[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]1([OH:12])[CH2:11][CH2:10][CH2:9]1

参加物

6

反応物 4

HCID 7912DiisopropylamineHCID 122863-BromopyridineHCID 14496CyclobutanoneHCID 178418339Butyllithium

生成物 1

HCID 68899458HCID 68899458、化合物収率 55.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3-bromopyridine (1 g, 6.329 mmol) was reacted with cylcobutanone (0.93 mL, 6.369 mmol), n-butyl lithium (4.02 mL, 7.64 mmol) and diisopropyl amine (0.99 mL, 7.005 mmol) in dry THF to afford the crude product. Purification by column chromatography on silica gel (40% ethyl acetate in hexane) afforded 802 mg of the product (55% yield). LCMS Purity: 79%, m/z=227.9 (M+1)

後処理

  1. customto afford the crude product
  2. customPurification by column chromatography on silica gel (40% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-b19ebe027a2343b88a28a1689e7387cc
出典データセット
uspto-grants-2016_05
特許番号
US09339501B2

反応ノート

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