홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

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

HRID 1633985
노트
인쇄 미리보기

반응식

HRID 1633985 반응식
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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 176Acetic AcidHCID 11430Potassium Carbonate2회HCID 574172Spiro[5.5]undecan-3-oneHCID 2729253Methyl 4-(aminomethyl)benzoate hydrochlorideHCID 5049666Sodium triacetoxyborohydride

생성물 1

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

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 962Water용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f5f891da2258402db015d59cb29a37be
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06503949B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트