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Triethylamine → HCID 86590533, 화합물

HRID 722272
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HRID 722272 반응식
[NH2:1][C@@H:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][C@@H:3]1[OH:11].C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>C1COCC1>[CH3:19][S:20]([NH:1][C@@H:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][C@@H:3]1[O:11][S:20]([CH3:19])(=[O:22])=[O:21])(=[O:22])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 2725045(1R,2S)-(+)-cis-1-Amino-2-indanol

생성물 1

HCID 86590533HCID 86590533, 화합물수율 93.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

(1R,2S)-1-Amino-2-hydroxyindan (3.0 g, 20mmol) was dissolved in dry THF (40 ml) and triethylamine (8.4 ml, 60.0 mmol) at 10° C. Methane sulphonyl chloride (5.0 g, 44.0 mmol) dissolved in THF (10 ml) was added at such a rate that the internal temperature remained below 15° C. Following the addition the mixture was stirred at room temperature for 20 hours and then evaporated. To the residue was added EtOAc (100 ml) and the mixture washed with saturated aqueous sodium bicarbonate and then water. The organic solution was dried over magnesium sulphate and evaporated to give (1R,2S)-1-methanesulphonamido-2-methylsulphonyloxyindan (5.7 g, 93%) as a pale yellow solid.

후처리

  1. customat 10° C
  2. additionwas added at such a rate that the internal temperature
  3. customremained below 15° C
  4. additionthe addition the mixture
  5. customevaporated
  6. additionTo the residue was added EtOAc (100 ml)
  7. washthe mixture washed with saturated aqueous sodium bicarbonate
  8. dry with materialThe organic solution was dried over magnesium sulphate
  9. customevaporated

출처 및 근거

ORD 기록
ord-5776be297d7a4a7bb609a747ebe23c39
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07138415B2

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