Water → Milveterol

HRID 226287노트

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HRID 226287 반응식
[OH:1][C@H:2]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:3][NH:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][NH:13][CH2:14][C@H:15]([OH:26])[C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[C:18]([NH:23][CH:24]=[O:25])[CH:17]=2)=[CH:7][CH:6]=1.[Cl:33]Cl.O>C(O)(C)C>[ClH:33].[OH:1][C@H:2]([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[CH2:3][NH:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][NH:13][CH2:14][C@H:15]([OH:26])[C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[C:18]([NH:23][CH:24]=[O:25])[CH:17]=2)=[CH:7][CH:6]=1.[OH:1][C@H:2]([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[CH2:3][NH:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][NH:13][CH2:14][C@H:15]([OH:26])[C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[C:18]([NH:23][CH:24]=[O:25])[CH:17]=2)=[CH:7][CH:6]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 24526ChlorineHCID 9892481Milveterol2회

생성물 2

HCID 9892481MilveterolHCID 11225217Milveterol hydrochloride

시약·촉매·용매 1

HCID 3776Isopropanol용매3회

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온도
5 °C

실험 절차

In a 250 mL flask a hydrochloride salt of compound 1 having 1.52 equivalents of chlorine per mole of compound 1 (5.0 g, 9.8 mmol) was suspended in 1:1 isopropanol:water (79 mL). The slurry was heated in a stepwise fashion, from 50° C. to 70° C. in 5° C. increments, to dissolve the solid. The solution was allowed to cool and isopropanol (80 mL) was added in one portion. Additional isopropanol (80 mL) was added dropwise and crystal formation was observed after about 75 mL was added. The slurry was stirred at room temperature for 16 h. The crystals were isolated by filtration, washed with cold 85% isopropanol/water (10 mL) followed by isopropanol (10 mL) and dried under vacuum to yield the monohydrochloride salt of compound 1.

후처리

  1. dissolutionto dissolve the solid
  2. temperatureto cool
  3. additionwas added
  4. customThe crystals were isolated by filtration
  5. washwashed with cold 85% isopropanol/water (10 mL)
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-2824ded7970147b19d8ec5b0980291e3
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557247B2

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