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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → HCID 22381731, 화합물

HRID 895775
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HRID 895775 반응식
[H-].[Na+].Cl[CH2:4][C:5]([NH:7][CH2:8][C:9]1[C:17]2[NH:16][C:15]3[CH2:18][CH2:19][CH2:20][C:14]=3[C:13]=2[CH:12]=[CH:11][CH:10]=1)=[O:6].O>CN(C=O)C>[CH2:4]1[N:16]2[C:17]3[C:13]([C:14]4[CH2:20][CH2:19][CH2:18][C:15]=42)=[CH:12][CH:11]=[CH:10][C:9]=3[CH2:8][NH:7][C:5]1=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24758Sodium hydrideHCID 22381724HCID 22381724, 화합물

생성물 1

HCID 22381731HCID 22381731, 화합물수율 58%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a suspension of NaH (124 mg, 3.10 mmol) in DMF (3 mL), 2-chloro-N-(1,2,3,4-tetrahydrocyclopenta[b]indol-5-ylmethyl)acetamide (135 mg, 0.515 mmol) in DMF (3 mL) was added at rt under Ar. After 16 h, H2O (2 mL) was added to quench the excess reagent, H2 evolved upon addition. After an additional 30 min, CHCl3 (20 mL) and H2O (10 mL) were added. The two layers were separated. The aqueous layer was extracted with CHCl3 (10 mL). The combined organic layers were dried over Na2SO4, filtered and concentrated in vacuo. Purification on SiO2, eluted with (30:1) CHCl3:CH3OH gave 67 mg (58%) of the title compound as a brown solid.

후처리

  1. additionwas added at rt under Ar
  2. customto quench the excess reagent, H2
  3. additionevolved upon addition
  4. waitAfter an additional 30 min
  5. additionCHCl3 (20 mL) and H2O (10 mL) were added
  6. customThe two layers were separated
  7. extractionThe aqueous layer was extracted with CHCl3 (10 mL)
  8. dry with materialThe combined organic layers were dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customPurification on SiO2
  12. washeluted with (30:1) CHCl3

출처 및 근거

ORD 기록
ord-73f05b65b1dc4cc28fe9f2f0fbe1d678
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06916922B2

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