Triethylamine → HCID 13079701, 화합물

HRID 2052506노트

반응식

HRID 2052506 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH2:17][OH:18])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>ClCCl>[CH3:26][S:27]([O:18][CH2:17][CH2:16][CH2:15][C:12]1[CH:11]=[CH:10][C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:14][CH:13]=1)(=[O:29])=[O:28]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 27640763-(4-(Benzyloxy)phenyl)propan-1-ol

생성물 1

HCID 13079701HCID 13079701, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
-10 °C

실험 절차

To a solution of 11.0 g. of 3-[p-(benzyloxy)phenyl]propanol and 10.4 ml. of triethylamine in 175 ml. of dichloromethane chilled to -10° C. is added dropwise, over 10 minutes, a solution of 3.89 ml. of methanesulfonyl chloride in 10 ml. of dichloromethane. The solution is stirred at -10° C. for 30 minutes, washed with 150 ml. of cold water, 75 ml. of cold 10% HCl, 75 ml. of cold saturated sodium bicarbonate, 75 ml. of cold saturated sodium chloride solution and dried over magnesium sulfate. The solvent is removed in vacuo to give off-white crystals, m.p. 65°-69° C.

후처리

  1. additionis added dropwise, over 10 minutes
  2. washwashed with 150 ml
  3. dry with materialof cold saturated sodium chloride solution and dried over magnesium sulfate
  4. customThe solvent is removed in vacuo
  5. customto give off-white crystals, m.p. 65°-69° C.

출처 및 근거

ORD 기록
ord-e3cf3379c8fe4bfaa9209066bf7c94ac
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04185115

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