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Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate → HCID 69639731、化合物

HRID 1792982
ノート
印刷プレビュー

反応式

HRID 1792982 の反応式
[CH2:1]([CH:3]([O:6][C:7]1[CH:8]=[C:9]([CH:20]=[CH:21][C:22](O)=[O:23])[CH:10]=[C:11]([O:14][CH:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[C:12]=1[OH:13])[CH2:4][CH3:5])[CH3:2].[CH3:25][C:26]1[CH:27]=[C:28]([CH2:33][CH2:34][CH2:35][NH2:36])[CH:29]=[CH:30][C:31]=1[CH3:32].F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>CN(C=O)C.CCN(CC)CC.C(Cl)Cl>[CH2:16]([CH:15]([O:14][C:11]1[CH:10]=[C:9]([CH:20]=[CH:21][C:22]([NH:36][CH2:35][CH2:34][CH2:33][C:28]2[CH:29]=[CH:30][C:31]([CH3:32])=[C:26]([CH3:25])[CH:27]=2)=[O:23])[CH:8]=[C:7]([O:6][CH:3]([CH2:1][CH3:2])[CH2:4][CH3:5])[C:12]=1[OH:13])[CH2:18][CH3:19])[CH3:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 108882543-(3,4-Dimethylphenyl)propan-1-amineHCID 69639651HCID 69639651、化合物

生成物 1

HCID 69639731HCID 69639731、化合物収率 90%

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒
HCID 6344
Dichloromethane
溶媒
HCID 8471Triethylamine溶媒

反応条件

温度
0 °C

実験手順

To the solution of 3-[3,5-bis-(1-ethylpropoxy)-4-hydroxyphenyl]acrylic acid (20 mg, 0.06 mmol) in DMF (0.2 ml) and Et3N (10 μl), was added 3(3,4-dimethylphenyl)propylamine (11 mg, 0.07 mmol) at 0° C. and was added the solution of BOP (29 mg, 0.07 mmol) in CH2Cl2 (0.2 ml). The solution was stirred for 30 minutes at 0° C. And then CH2Cl2 was evaporated in vacuo and the obtained residue was poured into ice water. The residue was extracted with EtOAc and washed with HCl (aq) and NaHCO3 (aq). And then the water was dried over anhydrous magnesium sulfate and filtered. The obtained filtrate was vacuum concentrated to give the residue, which was purified by column chromatography (EtOAc:Hexane=1:5), yielding 26 mg (90%) of the title compound as a oil.

後処理

  1. customAnd then CH2Cl2 was evaporated in vacuo
  2. additionthe obtained residue was poured into ice water
  3. extractionThe residue was extracted with EtOAc
  4. washwashed with HCl (aq) and NaHCO3 (aq)
  5. dry with materialAnd then the water was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give the residue, which
  9. customwas purified by column chromatography (EtOAc:Hexane=1:5)

出典と根拠

ORDレコード
ord-7feb93247a2c4c19a4a523417a2e1545
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07078407B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート