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Acetic Acid → 4-(Spiro[5.5]undec-3-ylaminomethyl)benzoic acid methyl ester

HRID 1633985
ノート
印刷プレビュー

反応式

HRID 1633985 の反応式
Cl.[CH3:2][O:3][C:4](=[O:13])[C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH2:12])=[CH:7][CH:6]=1.C(=O)([O-])[O-].[K+].[K+].C(O)(=O)C.[CH2:24]1[C:29]2([CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]2)[CH2:28][CH2:27][C:26](=O)[CH2:25]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCCl.O>[CH3:2][O:3][C:4](=[O:13])[C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH:12][CH:32]2[CH2:33][CH2:34][C:29]3([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]3)[CH2:30][CH2:31]2)=[CH:7][CH:6]=1
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

8

反応物 5

HCID 176Acetic AcidHCID 11430Potassium Carbonate2 回HCID 574172Spiro[5.5]undecan-3-oneHCID 2729253Methyl 4-(aminomethyl)benzoate hydrochlorideHCID 5049666Sodium triacetoxyborohydride

生成物 1

HCID 235501414-(Spiro[5.5]undec-3-ylaminomethyl)benzoic acid methyl ester

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

4-Aminomethylbenzoic acid methyl ester hydrochloride (1.45 g, 7.2 mmol) was suspended in 1,2-dichloroethane (50 mL) and added saturated aqueous potassium carbonate. The phases were separated and the aqueous layer was extracted with another portion of 1,2-dichloro-ethane (50 mL). The combined organic phases were added glacial acetic acid (435 μL, 7.6 mmol) followed by spiro[5.5]undecan-3-one (1.2 g, 7.2 mmol). The suspension was stirred for 30 min at 25° C. and sodium triacetoxyborohydride (2.27 g, 10.7 μmol) was added. After stirring for 2 days at 25° C., water (100 mL) and saturated aqueous potassium carbonate (15 mL) were added. The phases were separated and the aqueous layer was extracted with 1,2-di-chloroethane (2×100 mL). The combined organic phases were washed with water (100 mL) and brine (100 mL), dried over MgSO4 and evaporated to afford 4-(spiro[5.5]undec-3-ylaminomethyl)benzoic acid methyl ester which was used in the subsequent steps without further purification.

後処理

  1. customThe phases were separated
  2. extractionthe aqueous layer was extracted with another portion of 1,2-dichloro-ethane (50 mL)
  3. stirringAfter stirring for 2 days at 25° C.
  4. customThe phases were separated
  5. extractionthe aqueous layer was extracted with 1,2-di-chloroethane (2×100 mL)
  6. washThe combined organic phases were washed with water (100 mL) and brine (100 mL)
  7. dry with materialdried over MgSO4
  8. customevaporated

出典と根拠

ORDレコード
ord-f5f891da2258402db015d59cb29a37be
出典データセット
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06503949B1

反応ノート

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