Bromine → HCID 20374951、化合物

HRID 1448993

反応式

HRID 1448993 の反応式
[Na].[CH2:2]([O:9][C:10]1[CH2:14][CH:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:12][CH:11]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.BrBr.[CH3:25][NH:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]>C(O)CCCCCC.C1C=CC=CC=1>[CH2:27]([N:26]([CH3:25])[CH:12]1[CH:11]([O:9][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[CH:10]([O:9][CH2:2][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:14][CH:13]1[O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]

参加物

7

反応物 4

HCID 24408BromineHCID 93190N-MethylheptylamineHCID 5360545SodiumHCID 20374931HCID 20374931、化合物

生成物 1

HCID 20374951HCID 20374951、化合物

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回HCID 8129Heptanol溶媒

実験手順

0.23 g of sodium are dissolved in 30 ml of 1-heptanol at 50° under nitrogen. Dropwise, with stirring, there is added 4.88 g of N-heptyl-N-methyl-2-bromo-4,5-bibenzyloxycyclopentane-1-amine (obtainable from 3,5-dibenzyloxy-2-cyclopentene by the addition of bromine and reaction with 1-equivalent of methyl heptylamine), dissolved in 30 ml of benzene. Stirring is carried on for 6 hours at 50°. After cooling, 100 ml of benzene is added thereto. This is washed with water. The organic phase is dried over MgSO4 and the solvent is distilled off. After chromatographic purification of the residue (silica gel/chloroform:acetone=9:1), N-heptyl-N-methyl-5-heptyloxy-2,4-dibenzyloxy-cyclopentane-1-amine is obtained.

後処理

  1. stirringStirring
  2. customis carried on for 6 hours at 50°
  3. temperatureAfter cooling
  4. washThis is washed with water
  5. dry with materialThe organic phase is dried over MgSO4
  6. distillationthe solvent is distilled off
  7. customAfter chromatographic purification of the residue (silica gel/chloroform:acetone=9:1)

出典と根拠

ORDレコード
ord-94ef12ff946346dc905bfdf4177f9e32
出典データセット
uspto-grants-1980_02
特許番号
US04188403

関連ノート

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