1-Pentanethiol → HCID 19023126, 화합물

HRID 486381

반응식

HRID 486381 반응식
[H-].[Na+].[CH2:3]([SH:8])[CH2:4][CH2:5][CH2:6][CH3:7].[Na].[Cl:10][CH2:11][CH2:12][CH2:13]I>O1CCCC1>[CH2:3]([S:8][CH2:13][CH2:12][CH2:11][Cl:10])[CH2:4][CH2:5][CH2:6][CH3:7]

참가 물질

6

반응물 4

HCID 80671-PentanethiolHCID 24758Sodium hydrideHCID 813631-Chloro-3-iodopropaneHCID 5360545Sodium

생성물 1

HCID 19023126HCID 19023126, 화합물수율 59%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-78 °C

실험 절차

A suspension of sodium hydride (4.0 g, 100 mmole) in dry tetrahydrofuran (350 mL) under a nitrogen atmosphere was cooled in an ice bath. Pentyl mercaptan (10.8 g, 100 mmole) was added dropwise over 10 minutes. The resulting suspension of sodium alkylmercaptide was added in portions over 30 minutes to a stirred solution of 1-chloro-3-iodopropane (20.44 g, 100 mmole) in tetrahydrofuran (450 mL) that had been cooled to -78° C. The mixture was allowed to warm to ambient temperature overnight, then washed with brine, dried over MgSO4, and concentrated under vacuum. The resultant oil was distilled under water aspirator pressure to yield the desired product (10.67 g, 59% yield), b.p. 113°-119° C. (20 mm Hg).

후처리

  1. temperaturewas cooled in an ice bath
  2. temperatureto warm to ambient temperature overnight
  3. washwashed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under vacuum
  6. distillationThe resultant oil was distilled under water aspirator pressure

출처 및 근거

ORD 기록
ord-960bbc68ef3c4fda9453a5a236b22609
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292627

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