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Ammonium Chloride → 4-[4-chloro-1-(cyclopropylmethyl)-1H-benzotriazol-5-yl]benzyl methanesulfonate

HRID 2281071
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HRID 2281071 반응식
[Cl:1][C:2]1[C:10]2[N:9]=[N:8][N:7]([CH2:11][CH:12]3[CH2:14][CH2:13]3)[C:6]=2[CH:5]=[CH:4][C:3]=1[C:15]1[CH:20]=[CH:19][C:18]([CH2:21][OH:22])=[CH:17][CH:16]=1.C(N(CC)C(C)C)(C)C.[CH3:32][S:33](Cl)(=[O:35])=[O:34].[Cl-].[NH4+]>ClCCl>[CH3:32][S:33]([O:22][CH2:21][C:18]1[CH:17]=[CH:16][C:15]([C:3]2[CH:4]=[CH:5][C:6]3[N:7]([CH2:11][CH:12]4[CH2:14][CH2:13]4)[N:8]=[N:9][C:10]=3[C:2]=2[Cl:1])=[CH:20][CH:19]=1)(=[O:35])=[O:34]
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참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 31297Methanesulfonyl chloride2회HCID 81531DiisopropylethylamineHCID 70977671HCID 70977671, 화합물

생성물 1

HCID 867119864-[4-chloro-1-(cyclopropylmethyl)-1H-benzotriazol-5-yl]benzyl methanesulfonate

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

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온도
0 °C

실험 절차

{4-[4-Chloro-1-(cyclopropylmethyl)-1H-benzotriazol-5-yl]phenyl}methanol (0.71, 2.3 mmol) was dissolved in dichloromethane (7 mL) and treated with N,N-diisopropylethylamine (0.79 mL, 4.5 mmol). The mixture was cooled to 0° C. and treated with methanesulfonyl chloride (0.21 mL, 2.7 mmol) and after 1 hour, the mixture was treated with additional methanesulfonyl chloride (50 uL). After stirring for an additional 30 minutes, the mixture was poured into ammonium chloride (50 mL, aqueous saturated) and extracted with dichloromethane (2×100 mL). The combined organic extracts were dried with sodium sulfate, filtered and concentrated in vacuo, providing the titled compound.

후처리

  1. extractionextracted with dichloromethane (2×100 mL)
  2. dry with materialThe combined organic extracts were dried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-fe2047b710f14786a278a7737fce61d6
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09139576B2

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