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Triethylamine → HCID 59547800、化合物

HRID 1044493
ノート
印刷プレビュー

反応式

HRID 1044493 の反応式
[NH2:1][CH:2]1[CH:11]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([Cl:20])[CH:14]=2)[C:10]2[CH:9]=[C:8]([OH:21])[CH:7]=[CH:6][C:5]=2[CH2:4][CH2:3]1.C(N(CC)CC)C.[C:29](=O)([O:35]C(C)(C)C)[O:30][C:31]([CH3:34])([CH3:33])[CH3:32]>O1CCCC1>[Cl:20][C:15]1[CH:14]=[C:13]([CH:18]=[CH:17][C:16]=1[Cl:19])[CH2:12][CH:11]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([OH:21])[CH:9]=2)[CH2:4][CH2:3][CH:2]1[NH:1][C:29](=[O:35])[O:30][C:31]([CH3:34])([CH3:33])[CH3:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10219638Carbonic acid, bis(1,1-dimethylethyl) esterHCID 57471196HCID 57471196、化合物

生成物 1

HCID 59547800HCID 59547800、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

7-Amino-8-(3,4-dichlorobenzyl)-5,6,7,8-tetrahydronaphthalen-2-ol (10.8 g) and triethylamine (14.01 mL, 101 mmol) were dissolved in dry tetrahydrofuran (200 mL). Di-tert-butyl carbonate (7.31 g, 33.5 mmol) was added in small portions at room temperature. The reaction mixture was stirred over night. The solvent was evaporated in vacuo. The residue was dissolved in ethyl acetate (300 mL) and washed with water (2×200 mL). The ethyl acetate solution of the crude product was dried (Na2SO4). The solvent was evaporated in vacuo and the crude product was used for the next step without further purification. Yield: 12.2 g.

後処理

  1. customThe solvent was evaporated in vacuo
  2. dissolutionThe residue was dissolved in ethyl acetate (300 mL)
  3. washwashed with water (2×200 mL)
  4. dry with materialThe ethyl acetate solution of the crude product was dried (Na2SO4)
  5. customThe solvent was evaporated in vacuo
  6. customthe crude product was used for the next step without further purification

出典と根拠

ORDレコード
ord-052cf6c9da6e470796688e8a4096f345
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08563617B2

反応ノート

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