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Diethyl Ether → [4-(Chloromethyl)-1,3-thiazol-2-yl]methanol hydrochloride

HRID 1736659
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HRID 1736659 반응식
C([O:4][CH2:5][C:6]1[S:7][CH2:8][C:9]([CH2:12][Cl:13])(O)[N:10]=1)(=O)C.C(OCC)C>Cl.C(O)(C)C>[ClH:13].[Cl:13][CH2:12][C:9]1[N:10]=[C:6]([CH2:5][OH:4])[S:7][CH:8]=1
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참가 물질

5

반응물 2

HCID 3283Diethyl EtherHCID 117908272-Acetoxymethyl-4-chloromethyl-4-hydroxythiazoline

생성물 1

HCID 21464457[4-(Chloromethyl)-1,3-thiazol-2-yl]methanol hydrochloride수율 93%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 3776Isopropanol용매

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온도
0 °C

실험 절차

7.48 g of 2-acetoxymethyl-4-chloromethyl-4-hydroxythiazoline, prepared according to either Example 3 or 4, was suspended in 20 ml of 5N hydrogen chloride in isopropanol and heated to reflux for 45 minutes. The suspension was cooled in an ice bath and 30 ml of diethyl ether added dropwise over 30 minutes. The slurry was stirred a further 30 minutes at 0° C. and the precipitate filtered, washed with ether and dried under vacuum. 4-chloromethyl-2-hydroxymethylthiazole hydrochloride, 6.22 g (93% yield) was obtained.

후처리

  1. temperatureheated
  2. temperatureto reflux for 45 minutes
  3. temperatureThe suspension was cooled in an ice bath
  4. filtrationthe precipitate filtered
  5. washwashed with ether
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-3512514b84204a2a929dcc81f1bee325
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05541335

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